CN112029486A - Preparation method of environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer - Google Patents
Preparation method of environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer Download PDFInfo
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Abstract
The invention relates to the technical field of plugging and anti-sloughing agents for drilling fluid, in particular to a preparation method of an environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing filtrate reducer, which comprises the steps of adding humic acid, acrylic waste silk, water and strong base into a reaction kettle to react for 2-5 hours at the temperature of 30-160 ℃; transferring 20-30 parts by weight of the complex high molecular polymer into a reaction kettle, and reacting for 1-2 hours at 95-105 ℃; after the reaction, 3 to 3.8 parts of water, 2 to 5 parts of sodium metabisulfite, one or a mixture of sodium sulfite, 0.5 to 1 part of formaldehyde with the mass concentration of 30 to 40 percent and 0.2 to 0.8 part of phenol are added in sequence according to the parts by weight, and the mixture is reacted for 0.5 to 2.5 hours at the temperature of between 120 and 155 ℃; adding 15-25 parts of hydrolyzed polyacrylonitrile ammonium salt according to the parts by weight, and reacting for 0.5-1.5 hours at the temperature of 100-110 ℃; and drying to obtain a solid product. The product of the invention has the advantages of degradability, no secondary pollution, salt resistance and good high temperature resistance, and is widely suitable for deep well drilling under fresh water, 4% concentration salt water and pollution.
Description
Technical Field
The invention relates to the technical field of plugging and anti-sloughing agents for drilling fluid, in particular to a preparation method of an environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing filtrate reducer.
Background
Seventies, united states patent reports that the polymer fluid loss additive synthesized by phenol, urea, formaldehyde, sulfite and other modified components, namely, melamine, salicylic acid, benzoic acid and the like is not widely used due to the defects of difficult control of a synthesis method, high cost, poor temperature resistance and salt resistance and the like.
The patent with publication number CN85106524A developed in the eighties of China discloses a novel drilling mud treating agent containing humic acid and a preparation method thereof, wherein the method takes sodium sulfomethylhumate, sulfomethylphenolic resin and sulfomethyl hydrolysis polyacrylonitrile as raw materials, and prepares a product through a process route of normal pressure extraction, sedimentation slag discharge, evaporation concentration and graft polymerization with phenolic resin after sulfonation.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer, which has the advantages of high utilization rate of raw materials, no secondary pollution and low cost; good temperature and salt resistance, good viscosity reduction effect and improved rheological property.
The invention is realized by the following technical scheme:
a preparation method of an environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer comprises the following steps:
A. adding 30-68 parts of humic acid, 8-23 parts of acrylic fiber waste silk, 43-58 parts of water and 10-20 parts of strong base into a reaction kettle according to the parts by weight, and reacting for 2-5 hours at the temperature of 30-160 ℃;
B. transferring 20-30 parts by weight of the complex high molecular polymer into a reaction kettle, and reacting for 1-2 hours at 95-105 ℃;
C. after the reaction, 3 to 3.8 parts of water, 2 to 5 parts of sodium metabisulfite, one or a mixture of sodium sulfite, 0.5 to 1 part of formaldehyde with the concentration of 30 to 40 percent and 0.2 to 0.8 part of phenol are added in sequence according to the parts by weight to react for 0.5 to 2.5 hours at the temperature of between 120 and 155 ℃;
D. adding 15-25 parts of hydrolyzed polyacrylonitrile ammonium salt according to the parts by weight, and reacting for 0.5-1.5 hours at the temperature of 100-110 ℃;
E. and drying to obtain a solid product.
Preferably, the preparation method of the complex high molecular polymer comprises the following specific steps:
A. adding 35-58 parts of corn starch and 15-30 parts of liquid alkali with the mass concentration of 30% -40% into a kneader according to the parts by weight, and kneading and reacting for 0.3-1 hour at the temperature of 100-120 ℃;
B. after the reaction, 10-15 parts by weight of acetic acid is added into a kneader and reacted for 0.5-2.5 hours at the temperature of 120-145 ℃, and reactants are kneaded into particles.
Preferably, the content of the humic acid effective substances is 50-60%.
Preferably, the humic acid is weathered coal humic acid.
Preferably, the strong base is NaOH.
Preferably, the mass concentration of the formaldehyde is 36%.
Preferably, the liquid caustic soda has a mass concentration of 33%.
Preferably, the drying temperature in the step E is 200-300 ℃.
Compared with the prior art, the invention has the following advantages: the full-closed process is adopted, waste gas and waste residue are not produced, the utilization rate of raw materials is high, secondary pollution is not formed, and the cost is low; the temperature resistance and salt resistance are good, the viscosity reduction effect is good, and the rheological property is improved; the compatibility is good, and the paint can be matched with other treating agents for use, so that the comprehensive cost in drilling is reduced; the utilization of the waste acrylic fiber yarn as the raw material is waste utilization, has low price and sufficient supply, does not generate waste residues and waste gases during secondary utilization, is beneficial to environmental protection, can be degraded after alkalization, and greatly enhances the salt resistance.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example one
An environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer is prepared from the following raw materials in parts by weight:
20 parts of complex high molecular polymer, 30 parts of humic acid, 15 parts of hydrolyzed polyacrylonitrile ammonium salt, 8 parts of acrylic waste silk, 46 parts of water, 10 parts of NaOH, 2 parts of sodium metabisulfite, 0.5 part of formaldehyde solution with the mass concentration of 30% and 0.2 part of phenol. Wherein the complex high molecular polymer consists of 35 parts of corn starch, 15 parts of 30% liquid caustic soda and 10 parts of acetic acid; the content of humic acid effective components is 50%.
The preparation method of the complexing high-molecular polymer comprises the following specific steps:
A. adding the corn starch and 30% liquid alkali into a kneader to be kneaded and reacted for 1 hour at a high temperature of 100 ℃;
B. after the reaction, adding the acetic acid in parts by weight into a kneader, reacting for 0.5 hour at 135 ℃, observing the reaction condition, kneading the reactants into gray particles, and finishing other following operations for later use; the complex high molecular polymer uses common materials, so that the difficulty of production and purchase is reduced, the synthesis cost is reduced, and the complex high molecular polymer is convenient to popularize.
The preparation steps of the fluid loss agent are as follows:
A. adding the humic acid, the acrylic waste silk, the NaOH and 43 parts of water in parts by weight into a reaction kettle, and reacting for 5 hours at 30 ℃;
B. transferring the complex high molecular polymer in parts by weight to a reaction kettle, and stirring and reacting for 1 hour at 100 ℃;
C. after the reaction, the rest water, sodium metabisulfite, formaldehyde and phenol are added in turn according to the weight parts, and the reaction is carried out for 2.5 hours at the temperature of 120 ℃;
D. adding the hydrolyzed polyacrylonitrile ammonium salt in the weight portion according to the requirement, and reacting for 1.5 hours at the temperature of 100 ℃;
E. drying at the temperature of 200 ℃ to obtain a solid product, namely the environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer.
Example two
An environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer is prepared from the following raw materials in parts by weight:
the acrylic waste silk is utilized as a waste, has low price and sufficient supply, does not produce waste residues and waste gases during secondary utilization, is beneficial to environmental protection, can be degraded after alkalization, and greatly enhances the salt resistance. Wherein the complexing high molecular polymer consists of 58 parts of corn starch, 30 parts of liquid caustic soda with the mass concentration of 40% and 15 parts of acetic acid; the content of humic acid effective components is 60%.
The preparation method of the complexing high-molecular polymer comprises the following specific steps:
A. adding the corn starch and liquid alkali with the mass concentration of 40% in parts by weight into a kneader, kneading at a high temperature of 110 ℃ and rapidly reacting for 0.5 hour;
B. after the reaction, adding the acetic acid in parts by weight into a kneader, reacting for 2.5 hours at 120 ℃, observing the reaction condition, kneading the reactants into gray particles, and finishing the following operations for later use; the complex high molecular polymer uses common materials, so that the difficulty of production and purchase is reduced, the synthesis cost is reduced, and the complex high molecular polymer is convenient to popularize.
The preparation steps of the fluid loss agent are as follows:
A. adding the humic acid, the acrylic waste silk, the NaOH and 58 parts of water into a reaction kettle by weight for reacting for 2 hours at 160 ℃;
B. transferring the complex high molecular polymer in parts by weight into a reaction kettle, and slowly stirring and reacting for 2 hours at 105 ℃;
C. after the reaction, the rest water, sodium sulfite, formaldehyde and phenol are added in sequence, and the reaction is carried out for 0.5 hour at the temperature of 155 ℃;
D. adding the hydrolyzed polyacrylonitrile ammonium salt in the weight portion according to the requirement, and reacting for 0.5 hour at the temperature of 110 ℃;
E. drying at 300 deg.C to obtain solid product.
EXAMPLE III
The environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer is prepared from the following raw materials in parts by weight:
the acrylic waste silk is utilized as a waste, has low price and sufficient supply, does not generate waste residues and waste gases during secondary utilization, is beneficial to environmental protection, can be degraded after alkalization, and greatly enhances the salt resistance. Wherein the complexing high molecular polymer consists of 48 parts of corn starch, 20 parts of liquid caustic soda with the mass concentration of 33% and 12 parts of acetic acid; the content of humic acid effective substances is 60 percent.
The preparation method of the complexing high-molecular polymer comprises the following specific steps:
A. adding the corn starch and 33% liquid alkali into a kneader, kneading at 120 ℃ for rapid reaction for 0.3 hour;
B. after the reaction, acetic acid was added in the above-mentioned parts by weight to a kneader and reacted at 145 ℃ for 0.5 hour, and the reaction was observed and the reactants were kneaded into pellets for use.
A method for preparing an environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer comprises the following steps:
A. adding the humic acid, the acrylic waste silk, 45 parts of water and NaOH in parts by weight into a reaction kettle, and reacting for 2.5 hours at the temperature of 80 ℃;
B. transferring the complex high molecular polymer in parts by weight into a reaction kettle, and slowly stirring and reacting for 1.5 hours at 95 ℃;
C. after the reaction, the rest water, sodium sulfite, formaldehyde and phenol are added in turn according to the weight parts, and the reaction is carried out for 1.5 hours at 135 ℃;
D. adding the hydrolyzed polyacrylonitrile ammonium salt in the weight portion according to the requirement, and reacting for 1 hour at the temperature of 105 ℃;
E. drying at 250 ℃ to obtain a solid product.
The production process adopts a fully-closed process, does not produce waste gas and waste residue, has high utilization rate of raw materials, does not form secondary pollution, has low cost, good temperature and salt resistance and viscosity reduction effect, improves rheological property, has good compatibility, can be used together with other treating agents, reduces comprehensive cost in drilling, and is widely suitable for exploratory wells (without fluorescence) under fresh water, salt water or pollution.
The environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer has the following main performances measured by tests:
| sample and dosage | Measurement conditions | Apparent viscosity AV | Viscosity reduction rate | API dehydration ml | HTHP loss of water ml/30min |
| Fresh water base pulp | At room temperature | 59 | / | 25 | 70 |
| 3% filtrate reducer for fresh water base slurry | 180℃/16h | 20 | 79 | 5 | 22 |
| 4% NaCl-based slurry 5% filtrate reducer | 180℃/16h | 22 | 70 | 8 | 23 |
In-table detection method
Measuring 400ml of distilled water, adding 40g of soil for drilling fluid tests (SY 5490) and 1.4g of anhydrous sodium carbonate, stirring at a high speed for 20min, stopping twice in the stirring process to scrape off clay adhered to the wall of the container, then pouring the slurry into a sample cup, sealing and standing for 24h to obtain base slurry. Stirring the base slurry at high speed for 5min, measuring apparent viscosity by six-speed rotary viscosity, measuring API water loss by a medium-pressure filtration loss instrument, and measuring high-temperature high-pressure (HTHP) water loss by a high-temperature high-pressure filtration loss instrument.
Adding 12g of filtrate reducer into one part of 400ml of base slurry, stirring at a high speed for 20min, loading into a high-temperature tank, hot rolling for 16h at 180 ℃, cooling and taking out, stirring at a high speed for 5min, and measuring apparent viscosity, viscosity reduction rate, API (application program interface) filtrate loss and high-temperature high-pressure (HTHP) water loss according to GB/T16783.1-2006.
400mL of the slurry was taken, and 16.00g of sodium chloride (NaCl) was added thereto, respectively, and stirred at high speed for 20 min. Adding 20.00g (5%) of filtrate reducer, stirring at high speed for 20min, loading into a high-temperature tank, rolling at 180 ℃ for 16h, cooling, taking out, stirring at high speed for 5min, measuring apparent viscosity by using six-speed rotary viscosity after stirring at high speed for 5min, measuring API water loss by using a medium-pressure filtration instrument, and measuring high-temperature high-pressure (HTHP) water loss by using a high-temperature high-pressure filtration instrument.
From the above table, it can be seen that, without adding the present invention, the common freshwater base stock has 25ml of API dehydrated and 70ml/30min of HTHP dehydrated, and the addition of 3% of the present invention to the freshwater base stock can effectively reduce the dehydrated content, and after the present invention is added, particularly after the temperature is increased, the present invention can effectively reduce the apparent viscosity, has good viscosity reduction effect, improves the rheological property, has good compatibility, can be used in combination with other treating agents, reduces the comprehensive cost in drilling, and the waste silk of the acrylic fiber raw material has low price, is sufficient in supply, does not generate waste residue and waste gas during secondary utilization, is favorable for environmental protection, and can be degraded under the action of strong alkali. The apparent viscosity, API water loss and HTHP water loss of the present invention, using 5% in the 4% NaCl-based slurry, did not fluctuate much relative to the fresh water-based slurry, indicating that it greatly enhanced the salt and temperature resistance.
The production process adopts a fully-closed process, does not produce waste gas and waste residue, has high utilization rate of raw materials, does not form secondary pollution, has low cost, good temperature and salt resistance and viscosity reduction effect, improves rheological property, has good compatibility, can be used together with other treating agents, reduces comprehensive cost in drilling, and is widely suitable for exploratory wells (without fluorescence) under fresh water, salt water or pollution.
The present invention is not limited to the above-described embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention, and the contents of the changes still fall within the scope of the present invention.
Claims (8)
1. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse filtrate reducer is characterized by comprising the following steps: the method comprises the following steps:
A. adding 30-68 parts of humic acid, 8-23 parts of acrylic fiber waste silk, 43-58 parts of water and 10-20 parts of strong base into a reaction kettle according to the parts by weight, and reacting for 2-5 hours at the temperature of 30-160 ℃;
B. transferring 20-30 parts by weight of the complex high molecular polymer into a reaction kettle, and reacting for 1-2 hours at 95-105 ℃;
C. after the reaction, 3 to 3.8 parts of water, 2 to 5 parts of sodium metabisulfite, one or a mixture of sodium sulfite, 0.5 to 1 part of formaldehyde with the mass concentration of 30 to 40 percent and 0.2 to 0.8 part of phenol are added in sequence according to the parts by weight, and the mixture is reacted for 0.5 to 2.5 hours at the temperature of between 120 and 155 ℃;
D. adding 15-25 parts of hydrolyzed polyacrylonitrile ammonium salt according to the parts by weight, and reacting for 0.5-1.5 hours at the temperature of 100-110 ℃;
E. and drying to obtain a solid product.
2. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing fluid loss agent according to claim 1, wherein the preparation method comprises the following steps: the preparation method of the complex high molecular polymer comprises the following specific steps:
A. adding 35-58 parts of corn starch and 15-30 parts of liquid alkali with the mass concentration of 30% -40% into a kneader according to the parts by weight, and kneading and reacting for 0.3-1 hour at the temperature of 100-120 ℃;
B. after the reaction, 10-15 parts by weight of acetic acid is added into a kneader and reacted for 0.5-2.5 hours at the temperature of 120-145 ℃, and reactants are kneaded into particles.
3. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing fluid loss agent according to claim 1, wherein the preparation method comprises the following steps: the content of the humic acid effective substances is 50-60%.
4. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing fluid loss agent according to claim 3, wherein the preparation method comprises the following steps: the humic acid is weathered coal humic acid.
5. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing fluid loss agent according to claim 1, wherein the preparation method comprises the following steps: the strong base is NaOH.
6. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing fluid loss agent according to claim 1, wherein the preparation method comprises the following steps: the mass concentration of the formaldehyde is 36%.
7. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-collapse fluid loss agent according to claim 2, characterized in that: the mass concentration of the liquid caustic soda is 33%.
8. The preparation method of the environment-friendly degradable high-temperature-resistant salt-resistant anti-sloughing fluid loss agent according to claim 1, wherein the preparation method comprises the following steps: the drying temperature in the step E is 200-300 ℃.
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