CN112342002A - Descaling agent for sandstone acidification and preparation method thereof - Google Patents

Descaling agent for sandstone acidification and preparation method thereof Download PDF

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CN112342002A
CN112342002A CN202011221006.3A CN202011221006A CN112342002A CN 112342002 A CN112342002 A CN 112342002A CN 202011221006 A CN202011221006 A CN 202011221006A CN 112342002 A CN112342002 A CN 112342002A
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monomer
mixed solution
stirring
acidification
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徐克彬
祝琦
王中泽
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China National Petroleum Corp
CNPC Bohai Drilling Engineering Co Ltd
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Abstract

The invention discloses a scale remover for sandstone acidification and a preparation method thereof, wherein the scale remover is a polymer formed by copolymerizing a monomer A and a monomer B with the molar ratio of 1: 1; wherein the chemical structural formula of the monomer A is as follows:
Figure DDA0002761997880000011
the chemical structural formula of the monomer B is as follows:
Figure DDA0002761997880000012
the weight average molecular weight of the polymer is 1000-1300 g/mol, and the molecular weight distribution coefficient is 1.1-1.2; the descaling agent for sandstone acidification is a polymer containing sulfonic groups, can be directly added into the prepared acidification working solution for use, and can effectively remove calcium ions and magnesium ions in the acidification processWhen in use, the reaction or interaction between the acidizing working fluid and the acid-erodable minerals or acid-soluble substances is not influenced; in addition, the preparation method of the scale remover is simple, the scale remover is prepared by adding the initiator step by step at low temperature to initiate copolymerization, and the preparation cost is low, so that the scale remover has good marketization prospect.

Description

Descaling agent for sandstone acidification and preparation method thereof
Technical Field
The invention relates to the technical field of petroleum exploration and development, in particular to a scale remover for sandstone acidification and a preparation method thereof.
Background
The acidification is to dissolve the acid-erodible substances through the chemical reaction of hydrogen ions in the acid liquor and the acid-soluble substances in the stratum, thereby achieving the purposes of dredging and unblocking the obstructions in the stratum and improving the output of stratum substances. At present, the sandstone stratum is acidified by adopting earth acid. However, when the earth acid acidizes and erodes the sandstone stratum, calcium and magnesium ions are generated; when calcium and magnesium ions meet hydrofluoric acid in the earth acid, calcium fluoride and magnesium fluoride precipitates can be formed, so that sandstone pores are blocked, and the acidification effect is poor.
Disclosure of Invention
The invention aims to provide a scale remover for sandstone acidification, which can effectively remove calcium and magnesium ions in a sandstone formation in an acidification process.
The invention also aims to provide a preparation method of the descaling agent for sandstone acidification.
Therefore, the technical scheme of the invention is as follows:
a scale remover for sandstone acidification is characterized in that the scale remover is a polymer formed by copolymerizing a monomer A and a monomer B with a molar ratio of 1: 1; wherein the chemical structural formula of the monomer A is as follows:
Figure BDA0002761997860000011
the chemical structural formula of the monomer B is as follows:
Figure BDA0002761997860000012
the weight average molecular weight of the polymer is 1000-1300 g/mol, and the molecular weight distribution coefficient is 1.1-1.2.
The preparation method of the descaling agent for sandstone acidification comprises the following steps:
s1, adding the monomer A and the monomer B into deionized water, introducing nitrogen for protection in the process, and stirring at a shearing rate of 300r/min by using a shearing emulsifying stirrer to obtain a reaction mixed solution with uniform emulsion;
s2, introducing nitrogen for protection, heating the reaction mixed solution at a heating rate of 1 ℃/min to 40 ℃ at a stirring speed of 300r/min, adding a part of initiator after stirring for 5min, keeping the nitrogen protection, and stirring the mixed solution at a speed of 300r/min for 15 min;
s3, continuously heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 45 ℃, adding the rest initiator after stirring for 5min, keeping the protection of nitrogen and stirring the mixed solution at the speed of 500r/min for 15 min;
s4, after 15min, heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 50 ℃, stopping introducing nitrogen, and reacting for 6h under the stirring condition to obtain copolymer emulsion;
s5, stirring at the speed of 150r/min, and after the reaction liquid is naturally cooled to 45 ℃, removing the solvent water by rotary evaporation and placing the reaction liquid in an oven for drying to obtain a solid, namely the scale remover for sandstone acidification.
Preferably, in step S1, the ratio of the sum of the amounts of the monomer A and the monomer B to the volume of the ionized water is (0.6 to 1.20): 400.
Preferably, in the steps S1-S4, the pumping rate of the nitrogen protection is 0.2-0.3L/min.
Preferably, the initiator is a mixture of potassium persulfate and sodium bisulfite in a molar ratio of 1: 1;
preferably, the ratio of the amount of the initiator to the volume of the deionized water in the step S1 is 0.03-0.05: 100; wherein the amount of the initiator added for the first time in the step S3 is 1/4-1/3 of the total amount of the initiator.
Compared with the prior art, the descaling agent for sandstone acidification is a polymer containing sulfonic groups, can be directly added into the prepared acidification working solution for use, can effectively remove calcium and magnesium ions in the acidification process, and does not influence the reaction or interaction between the acidification working solution and acid-erodible minerals or acid-soluble substances; in addition, the preparation method is simple, the preparation cost is low, and the marketization prospect is good.
Drawings
FIG. 1 is a graph showing the relationship between the amount of water treatment agent added and the ion concentration in example 4 of the present invention.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, which are not intended to limit the invention in any way. In the following examples, monomers A and B are either available directly from commercial products or prepared in the laboratory itself; wherein, the chemical structural formula of A is as follows:
Figure BDA0002761997860000031
the liquid is liquid, can be directly weighed and then used in a dropwise manner during use, and the chemical structural formula of B is as follows:
Figure BDA0002761997860000032
the solid is dissolved in deionized water to prepare a solution of 1-3 mg/mL per time and then is dropwise added for use; the initiator is a mixture of potassium persulfate and sodium bisulfite in a molar ratio of 1: 1. The shearing emulsifying stirrer used in the step S1 adopts a model JRJ300-I stirrer of Shanghai Yuanmo electronic technology Limited; the weight average molecular weight of the copolymer was measured by GPC gel chromatography (the experimental apparatus is a gel chromatograph of the Wye corporation, USA, model number DAWNHELEOS II); the molecular weight distribution index is a ratio of the weight average molecular weight to the number average molecular weight measured by GPC gel chromatography.
Example 1
A scale remover for sandstone acidification is prepared by the following steps:
s1, adding 400mL of deionized water into a three-neck flask, then respectively dropwise adding 0.3mol of monomer A and 0.3mol of monomer B into the deionized water within 15min, introducing nitrogen into the three-neck flask at the speed of 0.3L/min for protection, and using a shearing emulsifying stirrer to make emulsion uniform at the shearing speed of 300r/min to obtain a reaction mixed solution;
s2, continuously introducing nitrogen into the three-neck flask at the speed of 0.3L/min for protection, heating the reaction mixed solution at the heating rate of 1 ℃/min under the stirring speed of 300r/min to 40 ℃, adding 0.03mol of initiator after stirring for 5min, continuously introducing nitrogen at the speed of 0.2L/min, and stirring the mixed solution at the speed of 300r/min for 15 min;
s3, continuously heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 45 ℃, adding the rest 0.09mol of initiator after stirring for 5min, introducing nitrogen at the speed of 0.3L/min, and stirring the mixed solution for 15min at the speed of 500 r/min;
s4, after 15min, heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 50 ℃, stopping introducing nitrogen, and reacting for 6h under the stirring condition to obtain copolymer emulsion;
s5, stirring at the speed of 150r/min, naturally cooling the reaction solution to 45 ℃, removing the solvent water by rotary evaporation, and drying in an oven to obtain 30.2g of solid, namely the sandstone acidification scale remover.
Through tests, the weight average molecular weight of the descaling agent for sandstone acidification is 1215g/mol, and the molecular weight distribution coefficient is 1.1; through the analysis of hydrogen spectrum and carbon spectrum of nuclear magnetic resonance, the molar ratio of the monomer A to the monomer B in the polymer is 1: 1; the infrared spectrum of the polymer shows that the polymer is 3040-3010 cm-1、1695～1540cm-1No characteristic peak exists at the position, which indicates that no carbon-carbon double bond exists, namely the monomer A and the monomer B form a polymer through polymerization reaction; it is 1650-1430 cm-1A characteristic peak of a benzene ring appears at the position, which indicates that the polymer contains the structure of the monomer B; it is between 1725 cm and 1700cm-1The presence of a carboxylic acid peak at the position indicates that monomer A is present in the polymer.
Example 2
A scale remover for sandstone acidification is prepared by the following steps:
s1, adding 400mL of deionized water into a three-neck flask, then respectively dropwise adding 0.4mol of monomer A and 0.4mol of monomer B into the deionized water within 15min, introducing nitrogen into the three-neck flask at the speed of 0.3L/min for protection, and using a shearing emulsifying stirrer to make emulsion uniform at the shearing speed of 300r/min to obtain a reaction mixed solution;
s2, continuously introducing nitrogen into the three-neck flask at the speed of 0.3L/min for protection, heating the reaction mixed solution at the heating rate of 1 ℃/min under the stirring speed of 300r/min to 40 ℃, adding 0.04mol of initiator after stirring for 5min, continuously introducing nitrogen at the speed of 0.3L/min, and stirring the mixed solution at the speed of 300r/min for 15 min;
s3, continuously heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 45 ℃, adding the rest 0.12mol of initiator after stirring for 5min, introducing nitrogen at the speed of 0.3L/min, and stirring the mixed solution for 15min at the speed of 500 r/min;
s4, after 15min, heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 50 ℃, stopping introducing nitrogen, and reacting for 6h under the stirring condition to obtain copolymer emulsion;
s5, stirring at the speed of 150r/min, naturally cooling the reaction solution to 45 ℃, removing the solvent water by rotary evaporation, and drying in an oven to obtain 39.6g of solid, namely the sandstone acidification descaling agent.
The weight average molecular weight of the descaling agent for sandstone acidification is 1255g/mol, and the molecular weight distribution coefficient is 1.2; through the analysis of hydrogen spectrum and carbon spectrum of nuclear magnetic resonance, the molar ratio of the monomer A to the monomer B in the polymer is 1: 1; the infrared spectrum of the polymer shows that the polymer is 3040-3010 cm-1、1695～1540cm-1No characteristic peak exists at the position, which indicates that no carbon-carbon double bond exists, namely the monomer A and the monomer B form a polymer through polymerization reaction; it is 1650-1430 cm-1A characteristic peak of a benzene ring appears at the position, which indicates that the polymer contains the structure of the monomer B; it is between 1725 cm and 1700cm-1The presence of a carboxylic acid peak at the position indicates that monomer A is present in the polymer.
Example 3
A scale remover for sandstone acidification is prepared by the following steps:
s1, adding 400mL of deionized water into a three-neck flask, then respectively dropwise adding 0.6mol of monomer A and 0.6mol of monomer B into the deionized water within 15min, introducing nitrogen into the three-neck flask at the speed of 0.3L/min for protection, and using a shearing emulsifying stirrer to ensure that emulsion is uniform at the shearing speed of 300r/min to obtain a reaction mixed solution;
s2, continuously introducing nitrogen into the three-neck flask at the speed of 0.3L/min for protection, heating the reaction mixed solution at the heating rate of 1 ℃/min under the stirring speed of 300r/min to 40 ℃, adding 0.05mol of initiator after stirring for 5min, continuously introducing nitrogen at the speed of 0.3L/min, and stirring the mixed solution at the speed of 300r/min for 15 min;
s3, continuously heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 45 ℃, adding the rest 0.15mol of initiator after stirring for 5min, introducing nitrogen at the speed of 0.3L/min, and stirring the mixed solution for 15min at the speed of 500 r/min;
s4, after 15min, heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 50 ℃, stopping introducing nitrogen, and reacting for 6h under the stirring condition to obtain copolymer emulsion;
s5, stirring at the speed of 150r/min, naturally cooling the reaction solution to 45 ℃, removing the solvent water by rotary evaporation, and drying in an oven to obtain 45.8g of solid, namely the sandstone acidification descaling agent.
Tests show that the weight average molecular weight of the descaling agent for sandstone acidification is 1285g/mol, and the molecular weight distribution coefficient is 1.2; through the analysis of hydrogen spectrum and carbon spectrum of nuclear magnetic resonance, the molar ratio of the monomer A to the monomer B in the polymer is 1: 1; the infrared spectrum of the polymer shows that the polymer is 3040-3010 cm-1、1695～1540cm-1No characteristic peak exists at the position, which indicates that no carbon-carbon double bond exists, namely the monomer A and the monomer B form a polymer through polymerization reaction; it is 1650-1430 cm-1A characteristic peak of a benzene ring appears at the position, which indicates that the polymer contains the structure of the monomer B; it is between 1725 cm and 1700cm-1The presence of a carboxylic acid peak at the position indicates that monomer A is present in the polymer.
The performance test was performed by taking the scale remover for sandstone acidizing prepared in example 3 as an example.
And (I) evaluating the compatibility of the acid by adopting a method for measuring acidity.
According to HCl + NaHCO3＝NaCl+H2O+CO2According to the reaction principle of ↓ and the ℃, when the consumption of hydrochloric acid is the same or results with close differences are obtained, the influence of the descaling agent for sandstone acidification on acid liquor can be judged to be small; since the effective component of the acid solution is hydrogen ions, the good compatibility with the acid solution can be shown as long as the effect on the hydrogen ions is proved.
Based on the above theory, first, 5 wt.% NaHCO was formulated3100mL each of the solution and 5 wt.% of dilute hydrochloric acid; then, 100mL of 5 wt.% diluted hydrochloric acid is poured into a 500mL beaker, the beaker is placed on a magnetic stirrer, and a magnetic stirrer is added to stir at the rotating speed of 100 r/min; next, a 100mL basic burette was filled with 5 wt.% NaHCO3The solution was added dropwise to dilute hydrochloric acid until no more bubbles were formed in the beaker. The measurements were performed 3 times in total and averaged. The test results are shown in table 1.
Table 1:
test items 1 2 3 Mean value of
NaHCO3Volume consumed/L 83.3 83.2 83.1 83.2
Pouring 100mL of 5 wt.% diluted hydrochloric acid into a 500mL beaker, weighing 1g of example 3, adding the diluted hydrochloric acid into the beaker, placing the beaker on a magnetic stirrer, adding a magnetic stirrer, and stirring at a rotating speed of 200r/min until the example 3 is completely dissolved; then, a 100mL basic burette was filled with 5 wt.% NaHCO3The solution was added dropwise to dilute hydrochloric acid until no more bubbles were formed in the beaker. The measurements were performed 3 times in total and averaged. The test results are shown in table 2 below.
Table 2:
test items 1 2 3 Mean value of
NaHCO3Volume consumed/L 83.1 83.1 83.2 83.2
Comparing the test results in tables 2 and 3, it can be seen that NaHCO was used in the test3The consumed volume difference is very small and almost consistent, so that the descaling agent for sandstone acidification has very small influence on hydrochloric acid and has good compatibility with acid.
If weak organic acid is used as working solution in acidification, the compatibility of the weak acid and the wetting reversal agent needs to be tested. Thus, 2 wt.% acetic acid was formulated using the same principles and the same tests as above were performed. The test results are shown in tables 3 and 4 below, respectively.
Table 3;
test items 1 2 3 Mean value of
NaHCO3volume/L of acetic acid consumed 55.8 56.1 55.7 55.9
Table 4:
Figure BDA0002761997860000071
comparing the test results in tables 2 and 3, it can be seen that NaHCO was used in the test3The consumed volume difference is 0.3mL, and the descaling agent for sandstone acidification has little influence on organic weak acid and good compatibility.
Example 4
The formation water of the region where the V1 well is located is MgCl2Water type, where it is locatedThe results of the water mineralization analysis of the layers are shown in table 5 below.
Table 5:
Figure BDA0002761997860000072
Figure BDA0002761997860000081
note: according to the water standard for preparing acid liquor, Ca2+、Mg2+The content of (A) should be less than 100 mg/L.
Respectively taking 20mL of formation water by a pipette, placing the formation water into 3 beakers, adding a stirrer, adding a calcium ion indicator, starting a multi-head magnetic stirrer, and stirring the formation water at the speed of 100 r/min; then 2 wt.% of the aqueous solution of example 3 was made up with distilled water and an acid burette was used to inject into the formation water until no calcium ions could be detected by the calcium ion electrode. The measurement was carried out three times in total, and the average value was taken.
Similarly, the magnesium ions were tested using the magnesium ion indicator using the same method as described above.
FIG. 1 is a graph showing the relationship between the dosage of the medium water treatment agent and the ion concentration. As can be seen from FIG. 1, the concentration of calcium and magnesium ions shows a clear trend of decreasing with the increasing dosage of the water treatment agent. At first, because the concentration of calcium and magnesium ions in formation water is high, a low-concentration water treatment agent cannot treat high-concentration calcium and magnesium ions after being added. Therefore, the water treatment agent is continuously added dropwise, but the concentration of calcium and magnesium ions is still high. With the continuous addition of the water treatment agent, a large amount of calcium and magnesium ions in the formation water are treated, the concentration of free calcium and magnesium ions remaining in the water is lower and lower, and the post-treatment speed is accelerated; finally, the removal rate of calcium and magnesium ions is more than or equal to 99 percent.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. A descaling agent for sandstone acidification is characterized in that the descaling agent is a polymer formed by copolymerizing a monomer A and a monomer B in a molar ratio of 1: 1; wherein the chemical structural formula of the monomer A is as follows:
Figure FDA0002761997850000011
the chemical structural formula of the monomer B is as follows:
Figure FDA0002761997850000012
the weight average molecular weight of the polymer is 1000-1300 g/mol, and the molecular weight distribution coefficient is 1.1-1.2.
2. The preparation method of the sandstone acidification descaling agent as claimed in claim 1, which is characterized by comprising the following steps:
s1, adding the monomer A and the monomer B into deionized water, introducing nitrogen for protection in the process, and stirring at a shearing rate of 300r/min by using a shearing emulsifying stirrer to obtain a reaction mixed solution with uniform emulsion;
s2, introducing nitrogen for protection, heating the reaction mixed solution at a heating rate of 1 ℃/min to 40 ℃ at a stirring speed of 300r/min, adding a part of initiator after stirring for 5min, keeping the nitrogen protection, and stirring the mixed solution at a speed of 300r/min for 15 min;
s3, continuously heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 45 ℃, adding the rest initiator after stirring for 5min, keeping the protection of nitrogen and stirring the mixed solution at the speed of 500r/min for 15 min;
s4, after 15min, heating the reaction mixed solution at the heating rate of 1 ℃/min to continuously heat the reaction mixed solution to 50 ℃, stopping introducing nitrogen, and reacting for 6h under the stirring condition to obtain copolymer emulsion;
s5, stirring at the speed of 150r/min, and after the reaction liquid is naturally cooled to 45 ℃, removing the solvent water by rotary evaporation and placing the reaction liquid in an oven for drying to obtain a solid, namely the scale remover for sandstone acidification.
3. The method for preparing the scale remover for sandstone acidification according to claim 2, wherein in step S1, the volume ratio of the sum of the amounts of the monomer A and the monomer B to the ionized water is (0.6-1.20): 400.
4. The method for preparing the descaling agent for sandstone acidification according to claim 2, wherein the pumping rate of the nitrogen protection in steps S1 to S4 is 0.2 to 0.3L/min.
5. The method for preparing the scale remover for sandstone acidification according to claim 2, wherein the initiator is a mixture of potassium persulfate and sodium bisulfite with a molar ratio of 1: 1.
6. The method for preparing the scale remover for sandstone acidification according to claim 2, wherein the ratio of the amount of initiator substances to the volume of the deionized water in the step S1 is 0.03-0.05: 100; wherein the amount of the initiator added for the first time in the step S3 is 1/4-1/3 of the total amount of the initiator.
CN202011221006.3A 2020-11-05 2020-11-05 Descaling agent for sandstone acidification and preparation method thereof Pending CN112342002A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1174817A (en) * 1996-03-01 1998-03-04 罗姆和哈斯公司 Method for metal sulfate scale control in Harsh oilfield conditions
US20090082535A1 (en) * 2005-03-31 2009-03-26 Nippon Shokubai Co., Ltd. (meth)acrylic acid copolymer, method for procucing the same, and application thereof
CN104119473A (en) * 2013-04-25 2014-10-29 墨西哥石油研究院 Process to obtain random copolymers derived from itaconic acid and/or its isomers and sodium alkenyl sulfonates and use of the product thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1174817A (en) * 1996-03-01 1998-03-04 罗姆和哈斯公司 Method for metal sulfate scale control in Harsh oilfield conditions
US20090082535A1 (en) * 2005-03-31 2009-03-26 Nippon Shokubai Co., Ltd. (meth)acrylic acid copolymer, method for procucing the same, and application thereof
CN104119473A (en) * 2013-04-25 2014-10-29 墨西哥石油研究院 Process to obtain random copolymers derived from itaconic acid and/or its isomers and sodium alkenyl sulfonates and use of the product thereof

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Application publication date: 20210209