CN111825795B - High-temperature fluid loss agent for well cementation and preparation method thereof - Google Patents

High-temperature fluid loss agent for well cementation and preparation method thereof Download PDF

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CN111825795B
CN111825795B CN202010736945.5A CN202010736945A CN111825795B CN 111825795 B CN111825795 B CN 111825795B CN 202010736945 A CN202010736945 A CN 202010736945A CN 111825795 B CN111825795 B CN 111825795B
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CN111825795A (en
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邱燮和
侯向前
赵继伟
何德瑞
尹海燕
代超玉
吴瑜
热依拉穆·依马穆
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Beijing Psv Petroleum Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52—Amides or imides
    • C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02—Well-drilling compositions
    • C09K8/03—Specific additives for general use in well-drilling compositions
    • C09K8/035—Organic additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract

The invention discloses a high-temperature fluid loss agent for well cementation and a preparation method thereof, wherein the preparation method comprises the steps of polymerizing a monomer, and forming the required fluid loss agent after aqueous solution of the polymerized monomer is polymerized and crosslinked; the polymerization monomers comprise, by mass, 40-60% of the monomer with the hydroxyl amide, 15-30% of the monomer with the acrylic acid and 20-40% of the functional monomer; the water loss reducing agent has double water loss reducing effects, on one hand, hydroxyl, carboxyl and sulfonic acid groups in the molecular structure of the water loss reducing agent have a complexing effect with cement calcium ions, and on the other hand, the carboxyl in the molecular structure of the water loss reducing agent has a complexing effect with a cross-linking agent zirconium ions, so that the water loss reducing effect can be exerted at the same time; has stronger function of preventing gas channeling; has certain retarding effect at high temperature, and can reduce the consumption of retarder at high temperature; the temperature resistance is excellent, and the highest temperature resistance can reach 240 ℃; the filtrate reducer has good salt resistance and meets the requirement of preparing cement slurry from seawater.

Description

High-temperature fluid loss agent for well cementation and preparation method thereof
Technical Field
The invention relates to the field of oilfield chemistry, and particularly relates to a high-temperature fluid loss agent for well cementation and a preparation method thereof.
Background
With the increasing demand of energy and the deepening of oil field exploration and development, the high-temperature deep well and ultra-deep well gradually become the focus of exploration and development. High temperature and ultrahigh temperature put higher requirements on the performance of the cement paste. The following difficulties mainly exist in the high-temperature deep well cementing process: (1) the water loss of the cement paste at high temperature and ultrahigh temperature is large and even uncontrollable, so that the construction safety risk exists; (2) the sedimentation stability of the cement slurry under high temperature and ultrahigh temperature is poor, and the solid phase is easy to subside in the pump stopping process, so that potential safety hazards are caused; (3) the cement slurry thickening time is difficult to adjust.
At present, the high molecular fluid loss additives mainly comprise high molecular polymers and synthetic high molecular polymers. The natural high molecular polymer comprises cellulose, cellulose derivatives, lignin, starch and other natural high molecular polymers with low price. Meanwhile, the problems of small adaptability of temperature range, poor product quality stability, easy degradation at high temperature and the like exist. The synthetic high molecular polymer comprises nonionic, anionic, cationic and zwitterionic polymers, and the synthetic high molecular fluid loss agent has various varieties and excellent performance, but has the defects of strong high-temperature dispersibility, too high viscosity of a slurry system, poor compatibility and influence on cement hydration reaction to reduce the cement strength.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the high-temperature fluid loss agent which has the advantages of low dosage, high temperature resistance, excellent fluid loss reduction performance, cement retardation and the like and has no influence on the strength of a well cementation cement slurry system, and the preparation method thereof.
The technical scheme adopted by the invention is as follows:
a high-temperature fluid loss agent for well cementation comprises a polymerization monomer, wherein the water solution of the polymerization monomer is polymerized and crosslinked to form the required fluid loss agent; the polymerization monomer comprises, by mass, 40-60% of a monomer with hydroxyl amide, 15-30% of an acrylic monomer and 20-40% of a functional monomer.
Further, the monomer with hydroxyl amide is one of N-hydroxymethyl acrylamide and N-hydroxyethyl acrylamide.
Further, the acrylic monomer is one of sodium acrylate and sodium methacrylate.
Further, the functional monomer is 3-allyloxy-2-hydroxy-1-propane sodium sulfonate.
Further, a molecular weight regulator is added before the polymerization reaction, and the molecular weight regulator is one of PEG200, PEG400 and PEG 600.
Further, after the molecular weight regulator is added, an initiator is added to initiate polymerization, wherein the initiator is one of ammonium persulfate and sodium persulfate.
Further, the method comprises the following step of adding a terminator to terminate the polymerization reaction after adding the initiator for a certain time, and adding one of sodium bisulfite and sodium thiosulfate.
Further, after the polymerization reaction is finished, a cross-linking agent is added for cross-linking reaction, wherein the cross-linking agent is lactic acid/glycerol organic zirconium.
A preparation method of a high-temperature fluid loss agent for well cementation comprises the following steps:
step 1: dissolving a polymerization monomer in water to form a solution A, and adjusting the pH to 5.0-6.0;
step 2: adding a molecular weight regulator into the solution A in the step 1 to form a solution B;
and step 3: adding an initiator into the solution B in the step 2 for polymerization;
and 4, step 4: adding a terminating agent into the solution after the polymerization is finished, and terminating the polymerization to form a polymer aqueous solution;
and 5: and (4) adding a cross-linking agent into the polymer aqueous solution formed in the step (4) for weak cross-linking, and cooling to form the required fluid loss agent.
Furthermore, the mass of the molecular weight regulator accounts for 0.1-1.2% of the mass of the polymerized monomer, the mass of the initiator accounts for 0.2-0.8% of the mass of the polymerized monomer, the molar mass ratio of the terminating agent to the initiator is 1:1, and the mass of the crosslinking agent accounts for 1.0-4.0% of the mass of the polymerized monomer.
The invention has the beneficial effects that:
(1) the fluid loss agent has double fluid loss reducing effects. On one hand, hydroxyl, carboxyl and sulfonic acid groups in the molecular structure of the fluid loss agent have a complexing effect on calcium ions in cement to form a certain structure, so that water is wrapped to play a fluid loss reducing effect; on the other hand, carboxyl in the water loss reducing molecular structure has a complexing effect with a cross-linking agent zirconium ion to form a net structure, and the compact net structure wraps water to play a water loss reducing effect;
(2) the water loss reducing agent has the function of preventing gas channeling, carboxyl in a water loss reducing molecular structure has a complexing effect with a cross-linking agent zirconium ion to form a compact network structure, and the water loss reducing agent can inhibit gas migration to a certain degree and play a role of preventing gas channeling.
(3) Carboxyl, hydroxyl and sulfonic acid groups in the molecular structure of the fluid loss agent have a complexing effect on calcium ions in cement, can inhibit cement hydration to a certain extent, has a certain retarding effect, can reduce the using amount of a retarder at high temperature, and saves cost;
(4) the fluid loss agent has excellent temperature resistance, and the temperature resistance can reach 240 ℃. Carboxyl and hydroxyl in the molecular structure of the fluid loss agent form a hydrogen bond structure similar to a network structure, so that the temperature resistance of the fluid loss agent is improved; meanwhile, carboxyl in the water loss reducing molecular structure has a complexing effect with a cross-linking agent zirconium ion to form a compact network structure, so that the temperature resistance of the water loss reducing agent is improved;
(5) the water loss reducing agent has good salt resistance effect and meets the requirement of preparing cement paste from seawater. The sulfonic acid group has strong hydration ability at high temperature, weak dehydration effect at high temperature and good solubility even in saturated saline.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention is further illustrated by the following specific examples.
A high-temperature fluid loss agent for well cementation comprises a polymerization monomer, wherein the water solution of the polymerization monomer is polymerized and crosslinked to form the required fluid loss agent; the polymerization monomer comprises, by mass, 40-60% of a monomer with hydroxyl amide, 15-30% of an acrylic monomer and 20-40% of a functional monomer. The mass concentration of the polymerization monomer in the polymerization monomer aqueous solution is 10-20%.
A preparation method of a high-temperature fluid loss agent for well cementation comprises the following steps:
step 1: dissolving a polymerization monomer in water to form a solution A, and adjusting the pH to 5.0-6.0;
step 2: adding a molecular weight regulator into the solution A in the step 1 to form a solution B;
and step 3: adding an initiator into the solution B in the step 2 for polymerization;
and 4, step 4: adding a terminating agent into the solution after the polymerization is finished, and terminating the polymerization to form a polymer aqueous solution;
and 5: and (4) adding a cross-linking agent into the polymer aqueous solution formed in the step (4) for weak cross-linking, and cooling to form the required fluid loss agent.
The monomer with hydroxyl amide is one of N-hydroxymethyl acrylamide and N-hydroxyethyl acrylamide. The acrylic monomer is one of sodium acrylate and sodium methacrylate. The functional monomer is 3-allyloxy-2-hydroxy-1-propane sodium sulfonate.
In the step 3, the polymerization temperature is 70-85 ℃, and preferably 75-80 ℃; the pH value is 5.0-6.0 in the polymerization process, and the polymerization time is 2-4 h, preferably 2-3 h; and 5, adding a cross-linking agent, and stirring for reaction for 0.5-1 h.
The molecular weight regulator is one of PEG200, PEG400 and PEG 600; the addition mass of the molecular weight regulator accounts for 0.1-1.2% of the mass of the polymerized monomer, and preferably 0.2-0.8%. The molecular weight regulator is a substance which is added in a polymerization system in a small amount and has a large chain transfer constant, can inform the molecular weight of a polymer and reduce the branching of a polymer chain, and mainly comprises aliphatic thiols, xanthic acid disulfides, polyhydric phenols, sulfur, halides and nitro compounds. PEG is creatively selected as a molecular weight regulator in the invention; PEG is not used as a precedent for a molecular weight regulator at present, and the PEG selected as the molecular weight regulator has very good effect in the invention.
The initiator is one of ammonium persulfate and sodium persulfate; the mass of the initiator added is 0.2-0.8%, preferably 0.4-0.5% of the mass of the polymerized monomer.
The terminating agent is one of sodium bisulfite and sodium thiosulfate; the molar ratio of the amount of the terminating agent to the amount of the initiator is 1: 1.
The cross-linking agent is lactic acid/glycerol organic zirconium. The mass of the cross-linking agent accounts for 1.0-4.0% of the mass of the polymerized monomer, and preferably 2.5-3.0%. The cross-linking agent may be referred to specifically as "organozirconium cross-linking AM/DMAM/AMPS terpolymer rheology".
The molecular weight of the fluid loss agent prepared by the invention is 20-80W.
Example 1
A preparation method of a high-temperature fluid loss agent for well cementation comprises the following steps:
step 1: 30.00g of 30.00g N-methylolacrylamide, 15.00g of sodium acrylate, 15.00g of sodium 3-allyloxy-2-hydroxy-1-propanesulfonate were dissolved in 230.00g of deionized water. The pH of the system was adjusted to 6.0.
Step 2: adding 0.1800g of PEG400, stirring uniformly, and transferring the solution into a 500mL three-neck flask;
and step 3: heating to 75 ℃ under the stirring condition of 100r/min, and dissolving 0.2401g of ammonium persulfate by using 5.00g of deionized water; dropping into a three-neck flask within 2min, and continuing to react for 2h at 75 ℃ after the dropping is finished.
And 4, step 4: dissolving 0.1095g of sodium bisulfite by 5.00g of deionized water, adding into a three-neck flask, continuing for 10min, and terminating polymerization to form a polymer aqueous solution;
and 5: and (4) adding 1.80g of lactic acid/glycerol organic zirconium cross-linking agent into the polymer aqueous solution formed in the step (4) for weak cross-linking, stirring for 0.5h, and cooling to form the required fluid loss agent.
The performance of the fluid loss agent prepared by the embodiment is tested and compared with the performance of the conventional fluid loss agent PVA 1788.
Preparing cement paste according to GB/T19139-: acksu G-grade cement, 35% of silicon powder, a fluid loss additive, a retarder and water, wherein the water-cement ratio is 0.44. The test results are shown in table 1, wherein the retarder is polymer SUP 304L.
Test procedure according to SY/T5504.2-2013 oil well cement external additive evaluation method part 2: and (4) reducing the loss of water.
TABLE 1 testing of fluid loss additives
Figure BDA0002605318440000041
Figure BDA0002605318440000051
From the table, under the condition that the addition amount of the fluid loss agent is the same and the experiment temperature is the same, compared with PVA1788, the fluid loss agent provided by the invention has the advantages that the API water loss amount is lower, and the fluid loss effect is better; the thickening time is obviously prolonged after the fluid loss is reduced by adding the fluid loss agent, which shows that the fluid loss agent prepared by the invention has a retarding effect at high temperature; compared with the method without adding the retarder, the method has the advantages that the water loss and the compressive strength of the API are not greatly different.
Gas channeling prevention property
Preparing cement paste according to GB/T19139-: acksu G-grade cement, 35% of silicon powder, a fluid loss additive, a retarder and water, wherein the water-cement ratio is 0.44. The test results are shown in table 1, wherein the retarder is polymer SUP 304L. And analyzing the gas channeling prevention performance of the fluid loss agent.
The SPN is one of the standards for measuring the gas channeling prevention capability of cement paste, and the larger the SPN is, the worse the gas channeling prevention capability is; conversely, the stronger the gas channeling prevention ability. The shorter the transition period of the cement paste from the beginning of initial setting (time of consistency 30BC in the expression) to the beginning of the solid state transition (time of consistency 100 BC), the greater the resistance of the cement paste. Experience has shown that: when SPN is more than 0 and less than or equal to 4, the gas channeling prevention capability is very strong.
SPN＝API*((t 100BC ) 1/2 -(t 30BC ) 1/2 )/(30) 1/2
TABLE 2 gas channeling prevention Performance test for fluid loss agent
Figure BDA0002605318440000052
From the table, the SPN values of the cement paste system are all less than 3 at different temperatures, which shows that the cement paste system has excellent gas channeling prevention capability, and shows that the fluid loss agent prepared by the invention has very strong gas channeling prevention capability.
Example 2
A preparation method of a high-temperature fluid loss agent for well cementation comprises the following steps:
step 1: 30.00g of 30.00g N-hydroxyethyl acrylamide, 18.00g of sodium methacrylate, 12.00g of sodium 3-allyloxy-2-hydroxy-1-propanesulfonate were dissolved in 530.00g of deionized water. The pH of the system was adjusted to 5.0.
Step 2: adding 0.0601g of PEG200, stirring uniformly, and transferring the solution to a 500mL three-neck flask;
and step 3: heating to 85 ℃ under the stirring condition of 100r/min, and dissolving 0.1200g of sodium persulfate by using 5.00g of deionized water; dropping into a three-neck flask within 2min, and continuing to react for 4h at 85 ℃ after the dropping is finished.
And 4, step 4: dissolving 0.1250g of sodium thiosulfate pentahydrate in 5.00g of deionized water, adding the solution into a three-neck flask, continuing for 10min, and terminating polymerization to form a polymer aqueous solution;
and 5: and (4) adding 1.20g of lactic acid/glycerol organic zirconium cross-linking agent into the polymer aqueous solution formed in the step (4) for weak cross-linking, stirring for 1h, and cooling to form the required fluid loss agent.
Example 3
A preparation method of a high-temperature fluid loss agent for well cementation comprises the following steps:
step 1: 27.00g of 27.00g N-methylolacrylamide, 9.00g of sodium acrylate, 24.00g of sodium 3-allyloxy-2-hydroxy-1-propanesulfonate were dissolved in 340.00g of deionized water. The pH of the system was adjusted to 5.5.
Step 2: adding 0.7200g of PEG200, stirring uniformly, and transferring the solution into a 500mL three-neck flask;
and step 3: heating to 80 ℃ under the stirring condition of 100r/min, and dissolving 0.4798g of ammonium persulfate by using 5.00g of deionized water; dropping into a three-neck flask within 2min, and continuing to react for 3h at 80 ℃ after the dropping is finished.
And 4, step 4: dissolving 0.2188g of sodium bisulfite by 5.00g of deionized water, adding into a three-neck flask, continuing for 10min, and terminating polymerization to form a polymer aqueous solution;
and 5: and (4) adding 0.60g of lactic acid/glycerol organic zirconium cross-linking agent into the polymer aqueous solution formed in the step (4) for weak cross-linking, stirring for 0.5h, and cooling to form the required fluid loss agent.
Example 4
A preparation method of a high-temperature fluid loss agent for well cementation comprises the following steps:
step 1: 24.00g of 24.00g N-methylolacrylamide, 12.00g of sodium acrylate, 24.00g of sodium 3-allyloxy-2-hydroxy-1-propanesulfonate were dissolved in 230.00g of deionized water. The pH of the system was adjusted to 5.5.
Step 2: 0.1202g of PEG400 is added and stirred evenly, and the solution is transferred into a 500mL three-neck flask;
and 3, step 3: heating to 75 ℃ under the stirring condition of 100r/min, and dissolving 0.2402g of ammonium persulfate by using 5.00g of deionized water; dropping into a three-neck flask within 2min, and continuing to react for 2h at 75 ℃ after the dropping is finished.
And 4, step 4: dissolving 0.1095g of sodium bisulfite by 5.00g of deionized water, adding into a three-neck flask, continuing for 10min, and terminating polymerization to form a polymer aqueous solution;
and 5: and (4) adding 1.50g of lactic acid/glycerol organic zirconium cross-linking agent into the polymer aqueous solution formed in the step (4) for weak cross-linking, stirring for 0.5h, and cooling to form the required fluid loss agent.
Example 5
A preparation method of a high-temperature fluid loss agent for well cementation comprises the following steps:
step 1: 36.00g of 36.00g N-methylolacrylamide, 9.00g of sodium acrylate, and 15.00g of sodium 3-allyloxy-2-hydroxy-1-propanesulfonate were dissolved in 230.00g of deionized water. The pH of the system was adjusted to 6.0.
Step 2: 0.4800g of PEG600 is added and stirred evenly, and the solution is transferred into a 500mL three-neck flask;
and step 3: heating to 75 ℃ under the stirring condition of 100r/min, and dissolving 0.3002g of ammonium persulfate by using 5.00g of deionized water; dropping into a three-neck flask within 2min, and continuing to react for 2h at 75 ℃ after the dropping is finished.
And 4, step 4: 0.1370g of sodium bisulfite is dissolved by 5.00g of deionized water, and is added into a three-neck flask to continue for 10min, and the polymerization is stopped to form a polymer aqueous solution;
and 5: and (4) adding 2.40g of lactic acid/glycerol organic zirconium cross-linking agent into the polymer aqueous solution formed in the step (4) for weak cross-linking, stirring for 0.5h, and cooling to form the required fluid loss agent.
The fluid loss agent has a certain retarding effect at high temperature, the consumption of the retarder can be reduced at high temperature, and the cost is saved; has stronger function of preventing gas channeling; the filtrate reducer has good salt resistance, meets the requirement of preparing cement paste by seawater, and has excellent temperature resistance up to 240 ℃; has double functions of reducing water loss.

Claims (4)

1. A high-temperature fluid loss agent for well cementation is characterized by comprising a polymerization monomer, wherein the required fluid loss agent is formed after aqueous solution of the polymerization monomer is polymerized and crosslinked; the polymerization monomers comprise, by mass, 40-60% of the monomer with the hydroxyl amide, 15-30% of the monomer with the acrylic acid and 20-40% of the functional monomer; the monomer with hydroxyl amide is one of N-hydroxymethyl acrylamide and N-hydroxyethyl acrylamide; the acrylic monomer is one of sodium acrylate and sodium methacrylate; the functional monomer is 3-allyloxy-2-hydroxy-1-propane sodium sulfonate; adding a molecular weight regulator before the polymerization reaction; after adding the molecular weight regulator, adding an initiator to initiate polymerization; after the polymerization reaction is terminated, adding a cross-linking agent for cross-linking reaction, wherein the cross-linking agent is lactic acid/glycerol organic zirconium; the molecular weight regulator is one of PEG200, PEG400 and PEG 600.
2. The high-temperature fluid loss agent for well cementation according to claim 1, wherein the initiator is one of ammonium persulfate and sodium persulfate.
3. The high-temperature fluid loss agent for well cementation according to claim 1, further comprising the step of adding a terminator to terminate the polymerization reaction after adding an initiator for a certain time, wherein the terminator is one of sodium bisulfite and sodium thiosulfate.
4. The preparation method of the high-temperature fluid loss agent for well cementation according to any one of claims 1 to 3, characterized by comprising the following steps:
step 1: dissolving a polymerization monomer in water to form a solution A, and adjusting the pH to 5.0-6.0;
step 2: adding a molecular weight regulator into the solution A in the step 1 to form a solution B;
and step 3: adding an initiator into the solution B in the step 2 for polymerization;
and 4, step 4: adding a terminating agent into the solution after the polymerization is finished, and terminating the polymerization to form a polymer aqueous solution;
and 5: adding a cross-linking agent into the polymer aqueous solution formed in the step 4 for weak cross-linking, and cooling to form the required fluid loss agent;
the mass of the molecular weight regulator accounts for 0.1-1.2% of the mass of the polymerized monomer, the mass of the initiator accounts for 0.2-0.8% of the mass of the polymerized monomer, the molar mass ratio of the terminating agent to the initiator is 1:1, and the mass of the cross-linking agent accounts for 1.0-4.0% of the mass of the polymerized monomer.
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