Composite synergistic discharge aiding agent and preparation method thereof

By adding sodium lignin sulfonate treated with directional enzymatic treatment to the composite efficiency discharge aid, ferric chloride and ferrous chloride that produce magnetic ferric tetroxide, the problem of particle aggregation of the discharge aid in high temperature and high salt environments is solved, efficient dispersion of the discharge aid and downhole magneto-controlled positioning of the discharge aid is achieved, and the oil and gas extraction efficiency is improved.

CN120209813AActive Publication Date: 2025-06-27SHAANXI BORUI PETROLEUM ENG TECH CO LTD

Patent Information

Application Number
CN202510700431.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-28
Publication Date
2025-06-27
Estimated Expiration
2045-05-28

AI Technical Summary

Technical Problem

In high-temperature and high-salt underground operation environments, existing discharge aids are prone to particle aggregation, reduced interface activity, deterioration of stability, and affecting mining efficiency.

Method used

By adding sodium lignin sulfonate, ferrous chloride, ferrous chloride and other components to the composite synergistic discharge aid, sodium lignin sulfonate is subjected to cellulase directed enzymatic treatment to improve the density and water solubility of the sulfonic acid group. Ferrous chloride and ferrous chloride react to generate magnetic ferrous tetraoxide to achieve downhole magnetocontrolled positioning.

Benefits of technology

Effectively inhibit particle aggregation, improve the water solubility and dispersion capacity of the discharge aid agent, improve its discharge rate and discharge aid performance in underground operations, and ensure the smooth exploitation of oil and gas.

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Abstract

The invention relates to the technical field of discharge aiding agents, in particular to a composite synergistic discharge aiding agent and a preparation method thereof. The composite synergistic discharge aiding agent is prepared from the following raw materials in percentage by weight: 6-10% of dodecyl dimethyl benzyl ammonium chloride, 2-4% of enzymolysis sodium lignin sulfonate, 1-3% of diethylenetriamine, 0.4-1.2% of a first additive, 0.2-0.4% of a second additive, 0.1-0.3% of a protective agent, 0.1-0.3% of a regulator and the balance of water. According to the invention, after the sodium lignin sulfonate is subjected to directional enzymolysis treatment by cellulase, the density of a sulfonic acid group is increased, the effect of inhibiting particle aggregation can be achieved, and meanwhile, residual cellulose in a molecular chain can be degraded, the molecular weight is reduced, and exposure of the sulfonic acid group is increased, so that the water solubility and the dispersing capacity of the sodium lignin sulfonate are improved; solid particles in a stratum can be better dispersed, pore channels are prevented from being blocked, and the use performance of the cleanup additive is effectively improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of drainage aids, and specifically provides a composite synergistic drainage aid and a preparation method thereof. Background Art

[0002] Drainage aids are chemical agents used in operations such as fracturing and acidizing of oil and gas wells. They can reduce the surface tension, decrease the capillary resistance, help the working fluids such as fracturing fluids and acid fluids to quickly drain from the formation, improve the flowback rate, reduce the damage to the formation, and thus increase the production and recovery rate of oil and gas wells.

[0003] In the prior art, as disclosed in Chinese Patent Publication No. CN101538462B, an oil well drainage aid is provided. The weight percentages of its components are as follows: dodecyldimethylbenzylammonium chloride: 7.5 - 13.5%; fatty alcohol polyoxyethylene ether: 2 - 3.5%; polyoxyethylene alkyl alcohol ether - 8: 25 - 34%; fatty alcohol polyoxyethylene ether: 3.5 - 5%; fluorocarbon surfactant FN - 3: 0.05 - 0.1%; the balance is water. Preparation method: Add fatty alcohol polyoxyethylene ether, JFC - 4, polyoxyethylene alkyl alcohol ether - 8, and fatty alcohol polyoxyethylene ether to an enamel reaction kettle in sequence according to the ratio. Heat up to 55 - 60 °C. First add 5% of water under stirring, add dodecyldimethylbenzylammonium chloride and fluorocarbon surfactant FN - 3 according to the ratio, stir for 30 minutes, then add water and cool to room temperature. It can reduce the adhesion force of the construction residue flowing in the reservoir, and accelerate the flowback of the residue by 20 - 30 percentage points.

[0004] In the prior art, in the downhole operation environment of oil and gas exploitation, the working state of high temperature and high salt will cause particles to easily aggregate, resulting in a decrease in the interfacial activity of the drainage aid and a deterioration in stability, which affects the exploitation efficiency. Based on this, the present invention provides a composite synergistic drainage aid and a preparation method thereof. Summary of the Invention

[0005] The purpose of the present invention is to provide a composite synergistic drainage aid and a preparation method thereof. The composite synergistic drainage aid prepared by the present invention not only has good drainage rate performance but also excellent drainage assistance rate performance, effectively improving the use performance of the drainage aid.

[0006] To achieve the above purpose, the present invention provides the following technical solutions: In the first aspect, the present invention provides a composite synergistic drainage aid, which comprises the following raw materials in weight percentages: 6 - 10% dodecyldimethylbenzylammonium chloride, 2 - 4% enzymatically hydrolyzed lignosulfonate, 1 - 3% diethylenetriamine, 0.4 - 1.2% first additive, 0.2 - 0.4% second additive, 0.1 - 0.3% protective agent, 0.1 - 0.3% regulator, and the balance is water; The raw materials of the first additive are composed of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol; The raw materials of the second additive are composed of ferric chloride and ferrous chloride, and the mass ratio of ferric chloride to ferrous chloride is 1:(3-4).

[0007] Furthermore, the enzymatically hydrolyzed lignosulfonate is prepared by the following method: lignosulfonate and cellulase are added to a water bath and mixed. The mass of the cellulase is 2-4% of the mass of the lignosulfonate. The water bath is set to heat up to 46-48 °C and keep warm for 20-30 h. The obtained product is washed and dried to obtain the enzymatically hydrolyzed lignosulfonate.

[0008] Furthermore, the mass ratio of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol is 10:(0.1-0.3):(0.1-0.3):(0.2-0.4).

[0009] Furthermore, the first additive is prepared by the following method: graphene oxide and N,N-dimethylformamide are added to a reaction kettle. The reaction kettle is set to heat up to 45-55 °C and keep warm and stir at 120-160 r / min for 6-10 min. Tetrahydrofuran is added during the stirring process. The obtained mixture is added to an ultrasonic disperser and ultrasonically treated for 10-20 min to obtain a mixed material. The mixed material and polyether polyol are added to a beaker, slowly stirred, and then left to react for 2-4 h. The obtained product is washed and dried to obtain the first additive.

[0010] Furthermore, the graphene oxide selected is a powder with a particle size of 0.1-1 μm.

[0011] Furthermore, both ferric chloride and ferrous chloride selected are powders with a particle size of 0.1-1 μm.

[0012] Furthermore, the second additive is prepared by the following method: ferric chloride and ferrous chloride are mixed evenly and then added to a water bath. Deionized water is added to the water bath, and the mass of the deionized water is 3-5 times the mass of the ferric chloride. The water bath is set to heat up to 60-70 °C, and at the same time, a stirring device is set to 100-200 r / min and keep warm and stir for 8-12 min. The stirred product is added to a reaction kettle, set to heat up to 80-90 °C, ammonia water is added, the pH is adjusted to 9-10, nitrogen is introduced into the reaction kettle, set to 600-800 r / min, and keep warm and stir for 10-20 min to obtain the second additive.

[0013] Furthermore, the protective agent is selected from any one of butylated hydroxytoluene, isothiazolinone, and silver ion antibacterial agent.

[0014] Further, the regulator is selected from any one of carboxymethyl cellulose and guar gum.

[0015] In a second aspect, the present invention also provides a preparation method of a composite synergistic drainage aid, comprising the following steps: S1: Weigh diethylenetriamine, a first additive and a second additive as required and add them into a mixer. 30% water is added to the mixer, and the mixer is set to stir at 500 - 700 r / min for 20 - 30 min to obtain a first premix. A regulator is added to the first premix, and the mixer is set to stir at 80 - 100 r / min for 4 - 6 min to obtain a second premix; S2: Add dodecyldimethylbenzylammonium chloride, enzymatically hydrolyzed lignosulfonate and a protective agent as required to the second premix, and add 70% water. Set the temperature to 40 - 50 °C, the rotation speed to 80 - 100 r / min, and the stirring treatment time to 20 - 60 min to prepare the composite synergistic drainage aid.

[0016] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. In the present invention, by adding the first additive and the second additive during the preparation of the composite synergistic drainage aid, wherein after the lignosulfonate is subjected to directional enzymatic hydrolysis by cellulase, the density of sulfonic acid groups is increased, which can play a role in inhibiting particle aggregation. At the same time, the residual cellulose in the molecular chain can be degraded, the molecular weight is reduced, and the exposure of sulfonic acid groups is increased, which improves its water solubility and dispersion ability, enables it to better disperse the solid particles in the formation, prevents the blockage of pore channels, and effectively improves the use performance of the drainage aid.

[0017] 2. In the present invention, magnetic iron tetroxide is generated by the reaction of ferric chloride and ferrous chloride in the second additive, which can realize downhole magnetic control positioning during the use of the drainage aid, effectively improve the sand-carrying capacity of the drainage aid, make the components of the second additive more evenly distributed in the downhole fractures, better maintain the fracture diversion channel, ensure the smooth exploitation of oil and gas, and further improve the use effect of the drainage aid. Specific embodiments

[0018] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0019] It should be noted that the raw materials used in the following embodiments are all commercially available raw materials.

[0020] Example 1:

[0021] A composite synergistic drainage aid, comprising the following raw materials by weight percentage: 6% dodecyldimethylbenzylammonium chloride, 2% enzymatically hydrolyzed lignosulfonate, 1% diethylenetriamine, 0.4% first additive, 0.2% second additive, 0.1% protective agent, 0.1% regulator; The raw materials of the first additive are composed of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol; The raw materials of the second additive are composed of ferric chloride and ferrous chloride, and the mass ratio of ferric chloride to ferrous chloride is 1:(3).

[0022] The enzymatically hydrolyzed lignosulfonate is prepared by the following method: lignosulfonate and cellulase are added to a water bath and mixed. The mass of cellulase is 2% of the mass of lignosulfonate. The water bath is set to heat up to 46 °C and keep warm for 20 h. The obtained product is washed and dried to obtain enzymatically hydrolyzed lignosulfonate.

[0023] The mass ratio of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol is 10:(0.1):(0.1):(0.2).

[0024] The first additive is prepared by the following method: graphene oxide and N,N-dimethylformamide are added to a reaction kettle. The reaction kettle is set to heat up to 45 °C and keep warm and stir at 120 r / min for 6 min. Tetrahydrofuran is added during the stirring process. The obtained mixture is added to an ultrasonic disperser and ultrasonically treated for 10 min to obtain a mixed material. The mixed material and polyether polyol are added to a beaker, slowly stirred and then left to react for 2 h. The obtained product is washed and dried to obtain the first additive.

[0025] The graphene oxide selected is a powder with a particle size of 0.1 μm.

[0026] Both ferric chloride and ferrous chloride are selected as powders with a particle size of 0.1 μm.

[0027] The second additive is prepared by the following method: ferric chloride and ferrous chloride are mixed evenly and then added to a water bath. Deionized water is added to the water bath, and the mass of deionized water is 3 times the mass of ferric chloride. The water bath is set to heat up to 60 °C, and at the same time, a stirring device is set at 100 r / min and kept warm and stirred for 8 min. The stirred product is added to a reaction kettle, set to heat up to 80 °C, ammonia water is added, the pH is adjusted to 9, nitrogen is introduced into the reaction kettle, set at 600 r / min, and kept warm and stirred for 10 min to obtain the second additive.

[0028] The protective agent selected is butylated hydroxytoluene.

[0029] The regulator selected is carboxymethyl cellulose.

[0030] A preparation method of a composite synergistic drainage aid, comprising the following steps: S1: Weigh diethylenetriamine, a first additive, and a second additive as required and add them to a mixer. Add 30% water to the mixer, set the mixer to stir at 500 r / min for 20 min to obtain a first premix. Add a regulator to the first premix, and set the mixer to stir at 80 r / min for 4 min to obtain a second premix; S2: Weigh dodecyldimethylbenzylammonium chloride, enzymatically hydrolyzed lignosulfonate, and a protective agent as required and add them to the second premix, and add 70% water. Set the temperature to 40 °C, the rotation speed to 80 r / min, and the stirring treatment time to 20 min to prepare the composite synergistic drainage aid.

[0031] Example 2:

[0032] A composite synergistic drainage aid, comprising the following raw materials by weight percentage: 8% dodecyldimethylbenzylammonium chloride, 3% enzymatically hydrolyzed lignosulfonate, 2% diethylenetriamine, 0.8% first additive, 0.3% second additive, 0.2% protective agent, 0.2% regulator; The raw materials of the first additive are composed of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol; The raw materials of the second additive are composed of ferric chloride and ferrous chloride, and the mass ratio of ferric chloride to ferrous chloride is 1:(3.5).

[0033] The enzymatically hydrolyzed lignosulfonate is prepared by the following method: lignosulfonate and cellulase are added to a water bath and mixed. The mass of cellulase is 3% of the mass of lignosulfonate. The water bath is set to heat up to 47 °C and keep warm for 25 h. The obtained product is washed and dried to prepare the enzymatically hydrolyzed lignosulfonate.

[0034] The mass ratio of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol is 10:(0.2):(0.2):(0.3).

[0035] The first additive is prepared by the following method: graphene oxide and N,N-dimethylformamide are added to a reaction kettle. The reaction kettle is set to heat up to 50 °C and keep warm and stir at 140 r / min for 8 min. Tetrahydrofuran is added during the stirring process. The obtained mixture is added to an ultrasonic disperser and ultrasonically treated for 15 min to obtain a mixed material. The mixed material and polyether polyol are added to a beaker, slowly stirred and then left to react for 3 h. The obtained product is washed and dried to prepare the first additive.

[0036] The graphene oxide selected is a powder with a particle size of 0.5 μm.

[0037] Both ferric chloride and ferrous chloride are selected as powders with a particle size of 0.5 μm.

[0038] The second additive is prepared by the following method: After mixing ferric chloride and ferrous chloride evenly, they are added to a water bath. Deionized water is added to the water bath, and the mass of the deionized water is 4 times that of the ferric chloride. The water bath is set to heat up to 65 °C, and at the same time, a stirring device is set at 150 r / min for heat preservation and stirring treatment for 10 min. The product obtained by stirring is added to a reaction kettle, set to heat up to 85 °C, ammonia water is added, the pH is adjusted to 9.5, nitrogen is introduced into the reaction kettle, set at 700 r / min, and heat preservation and stirring treatment is carried out for 15 min to obtain the second additive.

[0039] The preservative is selected as isothiazolinone.

[0040] The regulator is selected as guar gum.

[0041] A preparation method of a composite synergistic drainage aid includes the following steps: S1: Weigh diethylenetriamine, the first additive and the second additive as required and add them to a mixer. 30% water is added to the mixer, and the mixer is set to stir at 600 r / min for 25 min to obtain a first premix. The regulator is added to the first premix, and the mixer is set to stir at 90 r / min for 5 min to obtain a second premix; S2: Dodecyldimethylbenzylammonium chloride, enzymatically hydrolyzed lignosulfonate and a preservative are added to the second premix as required, and 70% water is added. The temperature is set at 45 °C, the rotation speed is 90 r / min, and the stirring treatment time is 40 min to obtain the composite synergistic drainage aid.

[0042] Example 3:

[0043] A composite synergistic drainage aid, comprising the following raw materials in weight percentages: 10% dodecyldimethylbenzylammonium chloride, 4% enzymatically hydrolyzed lignosulfonate, 3% diethylenetriamine, 1.2% the first additive, 0.4% the second additive, 0.3% preservative, 0.3% regulator; The raw materials of the first additive are composed of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol; The raw materials of the second additive are composed of ferric chloride and ferrous chloride, and the mass ratio of ferric chloride to ferrous chloride is 1:(4).

[0044] The enzymatically hydrolyzed lignosulfonate is prepared by the following method: Lignosulfonate and cellulase are added to a water bath and mixed. The mass of the cellulase is 4% of the mass of the lignosulfonate. The water bath is set to heat up to 48 °C and keep warm for 30 h. The obtained product is washed and dried to obtain the enzymatically hydrolyzed lignosulfonate.

[0045] The mass ratio of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol is 10:(0.3):(0.3):(0.4).

[0046] The first additive is prepared by the following method: Graphene oxide and N,N-dimethylformamide are added into a reaction kettle. The reaction kettle is set to heat up to 55°C and keep stirring at 160 r / min for 10 min. During the stirring process, tetrahydrofuran is added. The obtained mixture is added into an ultrasonic disperser and ultrasonically treated for 20 min to obtain a mixed material. The mixed material and polyether polyol are added into a beaker, slowly stirred, and then left to react for 4 h. The obtained product is washed and dried to obtain the first additive.

[0047] The graphene oxide selected is a powder with a particle size of 1 μm.

[0048] Both ferric chloride and ferrous chloride are selected as powders with a particle size of 1 μm.

[0049] The second additive is prepared by the following method: Ferric chloride and ferrous chloride are mixed evenly and then added into a water bath kettle. Deionized water is added into the water bath kettle, and the mass of the deionized water is 5 times that of the ferric chloride. The water bath kettle is set to heat up to 70°C, and at the same time, a stirring device is set to 200 r / min and keep stirring for 12 min. The stirred product is added into a reaction kettle, set to heat up to 90°C, ammonia water is added, and the pH is adjusted to 10. Nitrogen is introduced into the reaction kettle, set to 800 r / min, and keep stirring for 20 min to obtain the second additive.

[0050] The protective agent selected is a silver ion antibacterial agent.

[0051] The regulator selected is carboxymethyl cellulose.

[0052] A preparation method of a composite synergistic drainage aid includes the following steps: S1: Weigh diethylenetriamine, the first additive, and the second additive as required and add them into a mixer. 30% water is added into the mixer. The mixer is set to stir at 700 r / min for 30 min to obtain a first premixed material. The regulator is added into the first premixed material. The mixer is set to stir at 100 r / min for 6 min to obtain a second premixed material; S2: Add dodecyldimethylbenzylammonium chloride, enzymatically hydrolyzed lignosulfonate, and the protective agent as required into the second premixed material, and add 70% water. Set the temperature to 50°C, the rotation speed to 100 r / min, and the stirring treatment time to 60 min to prepare the composite synergistic drainage aid.

[0053] Comparative Example 1. The difference between this comparative example and Example 1 is that: In this comparative example, an equal amount of lignosulfonate is selected to replace the second additive.

[0054] Comparative Example 2: The difference between this comparative example and Example 1 is that this comparative example does not contain enzymatically hydrolyzed sodium lignosulfonate.

[0055] Comparative Example 3: The difference between this comparative example and Example 1 is that this comparative example does not contain the second additive.

[0056] Comparative Example 4: The difference between this comparative example and Example 1 is that this comparative example does not contain the first additive.

[0057] Performance test: Perform performance tests on the composite synergistic drainage aids prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4. The obtained test data are recorded in the following table:

[0058] In the performance test, referring to the test method in SY / T5755-2016, perform performance tests on the discharge rate and drainage aid rate of the composite synergistic drainage aids prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4.

[0059] It can be seen that the discharge rate performance and drainage aid rate performance of the composite synergistic drainage aids prepared in Comparative Examples 1, 2, 3, and 4 are lower than those in Examples 1, 2, and 3. This shows that: by adding the first additive and the second additive during the preparation of the composite synergistic drainage aid, among which, after the sodium lignosulfonate is subjected to directional enzymatic hydrolysis treatment by cellulase, the density of sulfonic acid groups is increased, which can play a role in inhibiting particle aggregation. At the same time, it can degrade the residual cellulose in the molecular chain, reduce the molecular weight, increase the exposure of sulfonic acid groups, which improves its water solubility and dispersion ability, enables it to better disperse the solid particles in the formation, prevent the blockage of pore channels, and effectively improve the use performance of the drainage aid. In the second additive, magnetic iron tetroxide is generated by the reaction of ferric chloride and ferrous chloride, which can realize downhole magnetic control positioning during the use of the drainage aid, effectively improve the sand-carrying capacity of the drainage aid, make the components of the second additive more evenly distributed in the downhole fractures, better maintain the fracture diversion channel, ensure the smooth exploitation of oil and gas, and further improve the use effect of the drainage aid.

[0060] By comparing and analyzing the relevant data in the table, it can be known that the composite synergistic drainage aid prepared by the present invention not only has good discharge rate performance but also excellent drainage aid rate performance. This shows that the composite synergistic drainage aid and its preparation method provided by the present invention have a broader market prospect and are more suitable for promotion.

[0061] In the description of this specification, the descriptions referring to the terms "one embodiment", "example", "specific example", etc. mean that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in a suitable manner in any one or more embodiments or examples.

[0062] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific embodiments described. Obviously, many modifications and variations can be made according to the content of this specification. These embodiments are selected and specifically described in this specification in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can well understand and utilize the present invention. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A composite synergistic drainage aid, characterized in that: It comprises the following raw materials by weight percentage: 6-10% dodecyldimethylbenzylammonium chloride, 2-4% enzymatically hydrolyzed sodium lignosulfonate, 1-3% diethylenetriamine, 0.4-1.2% first additive, 0.2-0.4% second additive, 0.1-0.3% protective agent, 0.1-0.3% regulator, and the balance is water; The raw materials of the first additive are composed of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol; The raw materials of the second additive are composed of ferric chloride and ferrous chloride, and the mass ratio of ferric chloride to ferrous chloride is 1:(3-4).

2. The composite synergistic drainage aid according to claim 1, characterized in that, The enzymatically hydrolyzed sodium lignosulfonate is prepared by the following method: sodium lignosulfonate and cellulase are added to a water bath and mixed. The mass of the cellulase is 2-4% of the mass of sodium lignosulfonate. The water bath is set to heat up to 46-48°C and kept warm for 20-30 h. The obtained product is washed and dried to obtain enzymatically hydrolyzed sodium lignosulfonate.

3. The composite synergistic drainage aid according to claim 1, wherein The mass ratio of graphene oxide, N,N-dimethylformamide, tetrahydrofuran, and polyether polyol is 10:(0.1-0.3):(0.1-0.3):(0.2-0.4).

4. The composite synergistic drainage aid according to claim 3, characterized in that, The first additive is prepared by the following method: graphene oxide and N,N-dimethylformamide are added to a reaction kettle. The reaction kettle is set to heat up to 45-55°C and kept warm and stirred at 120-160 r / min for 6-10 min. Tetrahydrofuran is added during the stirring process. The obtained mixture is added to an ultrasonic disperser and ultrasonically treated for 10-20 min to obtain a mixed material. The mixed material and polyether polyol are added to a beaker, slowly stirred and then allowed to stand and react for 2-4 h. The obtained product is washed and dried to obtain the first additive.

5. The composite synergistic drainage aid according to claim 3, wherein The graphene oxide selected is a powder with a particle size of 0.1-1 μm.

6. The composite synergistic drainage aid according to claim 1, wherein Both ferric chloride and ferrous chloride selected are powders with a particle size of 0.1-1 μm.

7. The composite synergistic drainage aid according to claim 6, characterized in that, The second additive is prepared by the following method: ferric chloride and ferrous chloride are mixed evenly and then added to a water bath. Deionized water is added to the water bath, and the mass of the deionized water is 3-5 times the mass of ferric chloride. The water bath is set to heat up to 60-70°C, and at the same time, a stirring device is set at 100-200 r / min and kept warm and stirred for 8-12 min. The stirred product is added to a reaction kettle, set to heat up to 80-90°C, ammonia water is added, the pH is adjusted to 9-10, nitrogen is introduced into the reaction kettle, set at 600-800 r / min, and kept warm and stirred for 10-20 min to obtain the second additive.

8. The composite synergistic drainage aid according to claim 1, wherein The protective agent selected is any one of butylated hydroxytoluene, isothiazolinone, and silver ion antibacterial agent.

9. The composite synergistic drainage aid according to claim 1, wherein The regulator selected is any one of carboxymethyl cellulose and guar gum.

10. A preparation method of the composite synergistic drainage aid according to any one of claims 1 to 9, characterized in that, It includes the following steps: S1: Weigh diethylenetriamine, the first additive, and the second additive as needed and add them into a mixer. Add 30% water into the mixer, set the mixer to stir at 500 - 700 r / min for 20 - 30 min to obtain a first premix. Add a regulator to the first premix, set the mixer to stir at 80 - 100 r / min for 4 - 6 min to obtain a second premix; S2: Weigh dodecyldimethylbenzylammonium chloride, enzymatically hydrolyzed lignosulfonate, and a protective agent as needed and add them into the second premix, and add 70% water. Set the temperature to 40 - 50 °C, the rotation speed to 80 - 100 r / min, and the stirring treatment time to 20 - 60 min to prepare a composite synergistic drainage aid.

Citation Information

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