A wax removal agent and preparation method thereof
By using heavy aromatics, lemon, polymethyl acrylic, fatty alcohol polyoxyethylene ether, modified methyl cellulose, and modified EVA in the waxing agent, it solves the difficulty removal of paraffin oil to block the existing technology The problem of effectively dissolving and dispersing the wax quality is achieved, preventing the solidification again, and ensuring the smooth progress of the oil collection process.
Patent Information
- Application Number
- CN202411602518.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-11
- Publication Date
- 2025-01-24
- Estimated Expiration
- 2044-11-11
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of oilfield exploitation, and in particular relates to a wax remover and a preparation method thereof. Background Art
[0002] Most of my country's oil fields are waxy crude oil. Before the development of oil wells, wax is completely dissolved in crude oil. During the oil well exploitation process, crude oil flows from the oil layer to the bottom of the well, and when it is lifted from the bottom of the well, as the temperature and pressure gradually decrease, paraffin forms crystals and precipitates and aggregates to form condensed wax blocks that adhere to the metal surface of the oil well facilities, affecting the normal production of the oil well. The wax blocks formed are mainly paraffin and microcrystalline wax, among which paraffin with normal alkanes as the main component is the majority. The wax deposition in oil wells is mainly affected by the wax content of crude oil, pressure, dissolved gas volume, wellbore lifting temperature difference, and pipe wall properties. Among them, the high crude oil content is an important internal cause of wax deposition. Therefore, in response to the wax deposition problem of high-wax oil wells, physical, chemical, and biological methods are often used for treatment. Chemical wax removal and prevention is widely used due to its simple process and low cost. However, the commonly used solvents with good wax removal performance are mainly carbon disulfide, carbon tetrachloride, benzene, toluene, gasoline, petroleum ether and other substances. These solvents have problems such as high toxicity, low flash point, and easy to cause poisoning of refining catalysts. Diesel or white oil is also used as a solvent, but the wax dissolving rate of diesel is low. Industrial white oil also has the problem of sulfur. In addition, after the existing wax remover dissolves the petroleum wax, it is easy to solidify into wax blocks again due to the influence of the formation conditions, which seriously affects the oil recovery process. Summary of the invention
[0003] In view of the above-mentioned prior art, the present invention provides a paraffin remover and a preparation method thereof to solve the technical problem that it is difficult to remove paraffin oil blockage in the prior art.
[0004] In order to achieve the above object, the technical solution adopted by the present invention is to provide a wax removal agent, comprising the following components in parts by weight:
[0005] 35-50 parts of heavy aromatics, 5-15 parts of limonene, 3-8 parts of polymethacrylate, 1-3 parts of fatty alcohol polyoxyethylene ether, 3-6 parts of modified methyl cellulose and 5-10 parts of modified EVA;
[0006] Modified methyl cellulose is prepared by the following steps:
[0007] S1: dissolving methylcellulose in water to prepare a solution with a concentration of 0.5-2 g / mL, and then adjusting the pH value of the resulting solution to 8-9;
[0008] S2: adding acrylic acid and initiator to the solution obtained in S1, and then reacting at 60-90°C for 12-16 hours in an inert atmosphere, and then adding terminator to terminate the reaction;
[0009] S3: Separate the product, wash it, and dry it to obtain the product;
[0010] The modified EVA is prepared by the following steps:
[0011] (1) mixing EVA resin, acrylate monomer and initiator in a mass ratio of 10:2-5:0.1-0.5 to obtain a mixed material;
[0012] (2) Add the mixed material into a melt extruder, control the screw speed to 10-15 r / min, the compression section temperature to 110-120°C, the homogenization section temperature to 135-140°C, the die temperature to 120-130°C, collect the extruded material and granulate it to obtain.
[0013] Based on the above technical solution, the present invention can also be improved as follows.
[0014] Further, the paraffin remover comprises the following components in parts by mass:
[0015] 40 parts of heavy aromatics, 10 parts of limonene, 5 parts of polymethacrylate, 2 parts of fatty alcohol polyoxyethylene ether, 5 parts of modified methyl cellulose and 8 parts of modified EVA (ethylene-vinyl acetate copolymer).
[0016] The beneficial effects of the present invention adopting the above technical solution are:
[0017] The present invention uses heavy aromatic hydrocarbons as the solvent of the wax removal agent. The heavy aromatic hydrocarbons have a relatively high boiling point and solubility, can exert a high solubility, and can effectively dissolve and remove wax deposits. In addition, the heavy aromatic hydrocarbons can give the wax solute a certain leveling property and wettability, thereby improving the dispersion performance of the wax solute. This property is also applicable to the wax removal process, and helps to remove the wax more thoroughly.
[0018] The wax remover of the present invention contains limonene, which, as a natural organic compound, has excellent solvent properties and can penetrate the structure of wax scale, destroy the attraction between its molecules, and make the wax scale loose and brittle, thereby being easier to dissolve and clean. In addition, limonene can also effectively decompose the chemical bonds of other stubborn dirt, making the wax blocks attached to the metal surface of oil well facilities easier to clean.
[0019] The paraffin remover of the present invention contains polymethacrylate, which can react with wax crystals precipitated from crude oil, and affect the growth direction and shape of wax crystals by adsorption or eutectic mode; specifically, polymethacrylate can inhibit the rapid growth of wax crystals in specific directions (such as the x-axis and the z-axis), and promote their growth in other directions (such as the y-axis), so that the precipitated wax crystals become equirectangular crystals with smaller particles and similar shapes, which helps to reduce the adhesion between wax crystals, delay or prevent the wax crystals from forming a three-dimensional network structure, and thus avoid the formation of wax blocks. In addition, polymethacrylate has good dissolving and dispersing ability, and it can effectively dissolve and disperse wax deposits, and peel them off from the surface or internal structure, so as to achieve the purpose of removing wax. The depressing effect of polymethacrylate combined with the dissolving and penetrating ability of limonene can effectively peel and dissolve the wax blocks, and will not solidify into wax blocks again, and can effectively remove the wax layer on the metal surface of oil well facilities.
[0020] The wax remover of the present invention contains fatty alcohol polyoxyethylene ether. As a nonionic surfactant, the fatty alcohol polyoxyethylene ether has excellent dispersing ability for dirt. In the wax removal process, it can disperse the wax dirt into smaller particles to prevent it from being re-deposited on the surface of the equipment, thereby improving the wax removal effect. In addition, the fatty alcohol polyoxyethylene ether molecules contain more oxyethylene units (obtained by addition of ethylene oxide), and these units can form hydrogen bonds or van der Waals forces with the molecules in the wax layer. The fatty alcohol polyoxyethylene ether has lower surface tension and good wetting properties. These characteristics enable the fatty alcohol polyoxyethylene ether to quickly reduce the tension between the liquid and the solid surface, so that the wax remover can more easily penetrate into tiny gaps and pores in the wax layer, thereby promoting the peeling and dissolution of the wax layer.
[0021] The paraffin remover of the present invention contains modified methyl cellulose, wherein the modified methyl cellulose is methyl cellulose grafted with acrylic acid. Methyl cellulose itself is a natural polysaccharide. After being grafted with acrylic acid, its solubility may be improved, so that the paraffin remover is more easily dispersed in water, thereby more effectively contacting and removing wax. Meanwhile, the introduction of acrylic acid into methyl cellulose may have better permeability, so that it can penetrate more deeply into waxy deposits and effectively peel off the wax layer attached to the metal surface. In addition, in the formation environment, the modified methyl cellulose can release acrylic acid and methyl cellulose, and the released acrylic acid can adjust the pH value of the system, dissolve dirt, and make the attached objects fall off more easily, while the methyl cellulose may provide better viscosity and stability, and prevent the fallen wax blocks and dirt from re-aggregating.
[0022] Modified EVA is also added to the paraffin remover of the present invention. The modified EVA used is acrylate-modified EVA. The acrylate-grafted modified EVA can affect the precipitation mode of wax in crude oil through its special grafting structure, increase the difficulty of wax precipitation, and thus avoid re-solidification of wax after the paraffin remover treatment.
[0023] The components in the wax remover of the present invention work synergistically, which can not only effectively peel off the wax layer on the metal surface, but also improve the solubility of the wax. After the wax is dissolved, it can be stably dispersed in the system without solidifying and aggregating again, which can effectively avoid the regeneration of wax blocks.
[0024] Furthermore, the heavy aromatics are at least one of isopropylbenzene, n-propylbenzene and ethyltoluene.
[0025] Furthermore, the polymethacrylate is polymethacrylate C18-22 alkyl ester (CAS#: 68459-84-7).
[0026] Furthermore, in S2, the mass ratio of acrylic acid and initiator to methyl cellulose is 2~5:0.1~0.5:10; the mass ratio of terminator to initiator is 1:1~3.
[0027] Furthermore, in S2, the initiator is ammonium persulfate; the terminator is sodium dimethyldithiocarbamate or sodium nitrite; and the inert atmosphere is nitrogen atmosphere.
[0028] Furthermore, in S2, the reaction temperature is 75° C. and the reaction time is 14 h.
[0029] Furthermore, in step (1), the initiator is tert-amyl peroxyneodecanoate or tert-butyl peroxypivalate.
[0030] Furthermore, in step (2), the screw speed is 12 r / min, the compression section temperature is 115° C., the homogenization section temperature is 135° C., and the die head temperature is 125° C.
[0031] The present invention also discloses a method for preparing the above-mentioned wax removal agent, comprising the following steps:
[0032] Add the formulated amount of limonene, polymethacrylate, fatty alcohol polyoxyethylene ether, modified methyl cellulose and modified EVA into heavy aromatic hydrocarbons, heat the mixture to 60-70° C., and stir for 3-5 hours to obtain the product.
[0033] The beneficial effects of the present invention are:
[0034] The components in the wax remover of the present invention work synergistically, which can not only effectively peel off the wax layer on the metal surface, but also increase the dissolution rate of the wax. After the wax is dissolved, it can be stably dispersed in the system without solidifying and aggregating again, which can effectively avoid the regeneration of wax blocks. DETAILED DESCRIPTION
[0035] The present invention will be described in detail below in conjunction with specific examples. The following examples are not intended to limit the present invention but are only intended to illustrate the present invention. The scope of the present invention is defined by the appended claims. The medicinal materials, reagents and reference substances used in the examples are purchased from the market unless otherwise specified.
[0036] Example 1
[0037] A paraffin remover, comprising the following components in parts by weight:
[0038] 40 parts of n-propylbenzene, 10 parts of limonene, 5 parts of polymethacrylate C18~22 alkyl ester (CAS#: 68459-84-7), 2 parts of fatty alcohol polyoxyethylene ether (AEO-9), 5 parts of modified methyl cellulose and 8 parts of modified EVA. Among them, the modified methyl cellulose is prepared by the following steps:
[0039] S1: dissolving methylcellulose in water to prepare a solution with a concentration of 0.1 g / mL, and then adjusting the pH value of the resulting solution to 8;
[0040] S2: Add acrylic acid and ammonium persulfate to the solution obtained in S1, then react at 75°C in a nitrogen atmosphere for 14 hours, and then add sodium nitrite to terminate the reaction; the mass ratio of the added acrylic acid and ammonium persulfate to the methyl cellulose is 3:0.3:10; the mass ratio of the added sodium nitrite to the ammonium persulfate is 1:1.
[0041] S3: Separate the product, wash it and dry it.
[0042] The modified EVA is prepared by the following steps:
[0043] (1) mixing EVA resin, acrylate monomer and tert-amyl peroxyneodecanoate in a mass ratio of 10:3:0.3 to obtain a mixture;
[0044] (2) Add the mixed material into a melt extruder, control the screw speed to 12 r / min, the compression section temperature to 115° C., the homogenization section temperature to 135° C., the die head temperature to 125° C., collect the extruded material and granulate it to obtain.
[0045] The paraffin remover in the present embodiment is prepared by following the steps:
[0046] Add the formulated amount of limonene, polymethacrylate C18-22 alkyl ester, fatty alcohol polyoxyethylene ether (AEO-9), modified methyl cellulose and modified EVA into n-propylbenzene, heat the mixture to 65°C, and stir for 4 hours to obtain the product.
[0047] Example 2
[0048] A paraffin remover, comprising the following components in parts by weight:
[0049] 35 parts of isopropylbenzene, 15 parts of limonene, 3 parts of polymethacrylate C18~22 alkyl ester (CAS#: 68459-84-7), 3 parts of fatty alcohol polyoxyethylene ether (AEO-9), 3 parts of modified methyl cellulose and 10 parts of modified EVA. Among them, the modified methyl cellulose is prepared by the following steps:
[0050] S1: dissolving methylcellulose in water to prepare a solution with a concentration of 0.5 g / mL, and then adjusting the pH value of the resulting solution to 8;
[0051] S2: Add acrylic acid and ammonium persulfate to the solution obtained in S1, then react at 60°C in a nitrogen atmosphere for 16 hours, and then add sodium dimethyldithiocarbamate to terminate the reaction; the mass ratio of the added acrylic acid and ammonium persulfate to methyl cellulose is 2:0.1:10; the mass ratio of the added sodium dimethyldithiocarbamate to ammonium persulfate is 1:2.
[0052] S3: Separate the product, wash it and dry it.
[0053] The modified EVA is prepared by the following steps:
[0054] (1) mixing EVA resin, acrylate monomer and tert-butyl peroxypivalate in a mass ratio of 10:2:0.1 to obtain a mixed material;
[0055] (2) Add the mixed material into a melt extruder, control the screw speed to 10 r / min, the compression section temperature to 120° C., the homogenization section temperature to 140° C., the die head temperature to 130° C., collect the extruded material and granulate it to obtain.
[0056] The paraffin remover in the present embodiment is prepared by following the steps:
[0057] Add the formulated amount of limonene, polymethacrylate C18-22 alkyl ester, fatty alcohol polyoxyethylene ether (AEO-9), modified methyl cellulose and modified EVA into cumene, heat the mixture to 60°C, and stir for 5 hours to obtain the product.
[0058] Example 3
[0059] A paraffin remover, comprising the following components in parts by weight:
[0060] 50 parts of ethyl toluene, 5 parts of limonene, 8 parts of polymethacrylate C18~22 alkyl ester (CAS#: 68459-84-7), 1 part of fatty alcohol polyoxyethylene ether (AEO-9), 6 parts of modified methyl cellulose and 5 parts of modified EVA. Among them, the modified methyl cellulose is prepared by the following steps:
[0061] S1: dissolving methylcellulose in water to prepare a solution with a concentration of 2 g / mL, and then adjusting the pH value of the resulting solution to 9;
[0062] S2: Add acrylic acid and ammonium persulfate to the solution obtained in S1, then react at 90°C in a nitrogen atmosphere for 12 hours, and then add sodium dimethyldithiocarbamate to terminate the reaction; the mass ratio of the added acrylic acid and ammonium persulfate to methyl cellulose is 5:0.5:10; the mass ratio of the added sodium dimethyldithiocarbamate to ammonium persulfate is 1:3.
[0063] S3: Separate the product, wash it and dry it.
[0064] The modified EVA is prepared by the following steps:
[0065] (1) mixing EVA resin, acrylate monomer and tert-butyl peroxypivalate in a mass ratio of 10:5:0.5 to obtain a mixed material;
[0066] (2) Add the mixed material into a melt extruder, control the screw speed to 15 r / min, the compression section temperature to 110° C., the homogenization section temperature to 135° C., the die head temperature to 120° C., collect the extruded material and granulate it to obtain.
[0067] The paraffin remover in the present embodiment is prepared by following the steps:
[0068] Add the formulated amount of limonene, polymethacrylate C18-22 alkyl ester, fatty alcohol polyoxyethylene ether (AEO-9), modified methyl cellulose and modified EVA into ethyl toluene, heat the mixture to 70°C, and stir for 3 hours to obtain the product.
[0069] Comparative Example 1
[0070] A paraffin remover, comprising the following components in parts by weight:
[0071] 40 parts of n-propylbenzene, 10 parts of limonene, 5 parts of polymethacrylate C18~22 alkyl ester (CAS#: 68459-84-7), 2 parts of fatty alcohol polyoxyethylene ether (AEO-9), 5 parts of methyl cellulose and 8 parts of modified EVA. The modified EVA is prepared by the following steps:
[0072] (1) mixing EVA resin, acrylate monomer and tert-amyl peroxyneodecanoate in a mass ratio of 10:3:0.3 to obtain a mixed material;
[0073] (2) Add the mixed material into a melt extruder, control the screw speed to 12 r / min, the compression section temperature to 115° C., the homogenization section temperature to 135° C., the die head temperature to 125° C., collect the extruded material and granulate it to obtain.
[0074] The paraffin remover in this comparative example is prepared by the following steps:
[0075] Add the formulated amount of limonene, polymethacrylate C18~22 alkyl ester, fatty alcohol polyoxyethylene ether (AEO-9), methyl cellulose and modified EVA into n-propylbenzene, heat the mixture to 65°C, and stir for 4 hours to obtain the product.
[0076] Comparative Example 2
[0077] A paraffin remover, comprising the following components in parts by weight:
[0078] 40 parts of n-propylbenzene, 10 parts of limonene, 5 parts of polymethacrylate C18~22 alkyl ester (CAS#: 68459-84-7), 2 parts of fatty alcohol polyoxyethylene ether (AEO-9), 5 parts of modified methyl cellulose and 8 parts of EVA. Among them, the modified methyl cellulose is prepared by the following steps:
[0079] S1: dissolving methylcellulose in water to prepare a solution with a concentration of 0.1 g / mL, and then adjusting the pH value of the resulting solution to 8;
[0080] S2: Add acrylic acid and ammonium persulfate to the solution obtained in S1, then react at 75°C in a nitrogen atmosphere for 14 hours, and then add sodium nitrite to terminate the reaction; the mass ratio of the added acrylic acid and ammonium persulfate to the methyl cellulose is 3:0.3:10; the mass ratio of the added sodium nitrite to the ammonium persulfate is 1:1.
[0081] S3: Separate the product, wash it and dry it.
[0082] The paraffin remover in the present embodiment is prepared by following the steps:
[0083] Add the formulated amount of limonene, polymethacrylate C18~22 alkyl ester, fatty alcohol polyoxyethylene ether (AEO-9), modified methyl cellulose and EVA into n-propylbenzene, heat the mixture to 65°C, and stir for 4 hours to obtain the product.
[0084] Comparative Example 3
[0085] A paraffin remover, comprising the following components in parts by weight:
[0086] 40 parts of n-propylbenzene, 10 parts of limonene, 5 parts of polymethacrylate C18~22 alkyl ester (CAS#: 68459-84-7), 2 parts of fatty alcohol polyoxyethylene ether (AEO-9), 5 parts of methyl cellulose and 8 parts of EVA.
[0087] The paraffin remover in this comparative example is prepared by the following steps:
[0088] Add the formulated amount of limonene, polymethacrylate C18~22 alkyl ester, fatty alcohol polyoxyethylene ether (AEO-9), methyl cellulose and EVA into n-propylbenzene, heat the mixture to 65°C, and stir for 4 hours to obtain the product.
[0089] Experimental example
[0090] Take petroleum wax from an oil field in Xinjiang, melt it and pour it into a mold to cool it, and take out the wax ball after it is fixed. Take 25mL of the wax remover obtained in the above embodiments and comparative examples respectively, and put it into different beakers, place the beaker in a constant temperature water bath and preheat it for 15 minutes, control the constant temperature water bath temperature at 45°C, and make the temperature of the wax remover consistent with the water bath temperature. Then put the wax ball of exactly the same specification (1g) into the wax remover, observe the dissolution state of the wax ball, until the wax ball is completely dissolved or the volume no longer changes, count the time taken for the wax ball to reach this state, and calculate the wax dissolution rate according to formula (1-1), the results are shown in Table 1.
[0091]
[0092] Wherein, v is the dissolution rate, in g / min; m is the mass of the wax ball (the wax ball dissolved in the wax remover), in g; t is the time taken for the wax ball to be completely dissolved, in min.
[0093] Table 1 Wax dissolving rate of different wax removal agents
[0094] Final state of the wax ball Wax dissolving rate (g / min) Example 1 Completely dissolved, no solid precipitation at the bottom of the cup 0.72 Example 2 Completely dissolved, no solid precipitation at the bottom of the cup 0.69 Example 3 Completely dissolved, no solid precipitation at the bottom of the cup 0.70 Comparative Example 1 A small amount of residue, no solid precipitation at the bottom of the cup 0.45 Comparative Example 2 Completely dissolved, solid precipitation appears at the bottom of the cup 0.42 Comparative Example 3 Some residue, solid precipitation appears at the bottom of the cup 0.17
[0095] As can be seen from Table 1, the use of the intermediate wax clearing agent of the present invention (Examples 1 to 3) can make petroleum wax dissolve faster, and after the petroleum wax is dissolved, the wax is stably dispersed in the dissolution system, and there will be no problem of wax re-aggregation and solidification. Compared with Example 1, the methyl cellulose used in Comparative Example 1 has not been modified, and the wax balls cannot be dissolved well, resulting in a slow dissolution rate of the wax balls and inability to dissolve completely. Compared with Example 1, the EVA used in Comparative Example 2 has not been modified, and the wax precipitation cannot be well prevented. The dissolved wax is easy to re-precipitate and re-form a wax layer. Compared with Example 1, the methyl cellulose and EVA used in Comparative Example 3 have not been modified, and the dissolution rate and dissolution effect of the wax balls are significantly adversely affected.
[0096] Although the specific implementation of the present invention is described in detail in conjunction with the embodiments, it should not be understood as limiting the scope of protection of this patent. Within the scope described in the claims, various modifications and variations that can be made by those skilled in the art without creative work still fall within the scope of protection of this patent.
Claims
1. A paraffin remover, characterized in that: The composition comprises the following components in parts by weight: 35-50 parts of heavy aromatics, 5-15 parts of limonene, 3-8 parts of polymethacrylate, 1-3 parts of fatty alcohol polyoxyethylene ether, 3-6 parts of modified methyl cellulose and 5-10 parts of modified EVA; The modified methyl cellulose is prepared by the following steps: S1: dissolving methylcellulose in water to prepare a solution with a concentration of 0.5-2 g / mL, and then adjusting the pH value of the resulting solution to 8-9; S2: adding acrylic acid and initiator to the solution obtained in S1, and then reacting at 60-90°C for 12-16 hours in an inert atmosphere, and then adding terminator to terminate the reaction; S3: Separate the product, wash it, and dry it to obtain the product; The modified EVA is prepared by the following steps: (1) mixing EVA resin, acrylate monomer and initiator in a mass ratio of 10:2-5:0.1-0.5 to obtain a mixed material; (2) Add the mixed material into a melt extruder, control the screw speed to 10-15 r / min, the compression section temperature to 110-120°C, the homogenization section temperature to 135-140°C, the die temperature to 120-130°C, collect the extruded material and granulate it to obtain.
2. The paraffin remover according to claim 1, characterized in that: The composition comprises the following components in parts by weight: 40 parts of heavy aromatic hydrocarbons, 10 parts of limonene, 5 parts of polymethacrylate, 2 parts of fatty alcohol polyoxyethylene ether, 5 parts of modified methyl cellulose and 8 parts of modified EVA.
3. The paraffin remover according to claim 1 or 2, characterized in that: The heavy aromatic hydrocarbon is at least one of isopropylbenzene, n-propylbenzene and ethyltoluene.
4. The paraffin remover according to claim 1 or 2, characterized in that: The polymethacrylate is polymethacrylate C18-22 alkyl ester.
5. The paraffin remover according to claim 1, characterized in that: The mass ratio of the acrylic acid and the initiator to the methyl cellulose in S2 is 2-5:0.1-0.5:10; the mass ratio of the terminator to the initiator is 1:1-3.
6. The paraffin remover according to claim 1 or 5, characterized in that: In S2, the initiator is ammonium persulfate; the terminator is sodium dimethyldithiocarbamate or sodium nitrite; and the inert atmosphere is nitrogen atmosphere.
7. The paraffin remover according to claim 1, characterized in that: The reaction temperature in S2 is 75°C and the reaction time is 14h.
8. The paraffin remover according to claim 1, characterized in that: The initiator in step (1) is tert-amyl peroxyneodecanoate or tert-butyl peroxypivalate.
9. The paraffin remover according to claim 1, characterized in that: In step (2), the screw speed is 12 r / min, the compression section temperature is 115° C., the homogenization section temperature is 135° C., and the die head temperature is 125° C.
10. The method for preparing the paraffin removal agent according to any one of claims 1 to 9, characterized in that: The following steps are involved: Add the formulated amount of limonene, polymethacrylate, fatty alcohol polyoxyethylene ether, modified methyl cellulose and modified EVA into heavy aromatic hydrocarbons, heat the mixture to 60-70° C., and stir for 3-5 hours to obtain the product.
Citation Information
Patent Citations
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