CN115466337A - Modified temperature-resistant salt-resistant guanidine gum containing conjugated groups and preparation method thereof - Google Patents
Modified temperature-resistant salt-resistant guanidine gum containing conjugated groups and preparation method thereof Download PDFInfo
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Abstract
The invention relates to modified temperature-resistant salt-resistant guanidine gum containing conjugate groups, which has the following structural formula:
the preparation method comprises the following steps: SN reaction of aminoethanesulfonic acid with cyanuric chloride 2 Performing nucleophilic substitution reaction to obtain a chlorinated etherifying agent with surface activity, dissolving the chlorinated etherifying agent in an alcohol-water solvent to prepare a chlorinated etherifying agent solution, performing an alkalization reaction on the guar gum in the alcohol-water solvent, adding the chlorinated etherifying agent solution to perform an etherification reaction, and filtering, washing, neutralizing, drying, crushing and sieving the product to obtain the surfactant modified guar gum. The invention has reliable principle and simple and convenient operation, and introduces the surface active agent of sulfonic acid group and six-membered ring into guanidine gum moleculeThe structure improves the dissolution, salt tolerance and temperature tolerance of the guanidine gum, and has wide market application prospect.
Description
Technical Field
The invention relates to a modified temperature-resistant salt-resistant guanidine gum containing a conjugated group and a preparation method thereof, belonging to the field of oilfield production increasing measures.
Background
In western regions and offshore areas of China, due to shortage of fresh water resources, flowback stratum water with high salinity and seawater are used as local materials for large-scale fracturing operation, and higher requirements on the temperature resistance of a fracturing fluid are provided along with continuous rise of the temperature of an exploration and development reservoir stratum, so that the temperature resistance and salt resistance of the guanidine gum fracturing fluid are improved, the development requirements of the saline water preparation and the high-temperature reservoir stratum are met, and the guanidine gum fracturing fluid has important practical significance.
Guanidine gum is used as a thickening agent, under the condition of high mineralization degree, because different types of cations are contained, the cations neutralize negative charges on polymer chains, so that the repulsive force between the polymer chains is reduced, the polymer chains cannot be fully stretched in an aqueous solution, the molecular chain winding probability is reduced, the viscosity of the polymer solution is greatly reduced, and the hydration and the thickening of the guanidine gum are influenced. At high temperatures, the cleavage of glycosidic bonds in the backbone leads to a decrease in molecular weight and destruction of the polymer structure, losing thermal stability and thermal reversibility. Therefore, the grafted salt-resistant and temperature-resistant groups are chemically modified by the guanidine gum, and the improvement of the structural strength and the temperature resistance of the guanidine gum molecules is particularly important. At present, many scholars research salt-resistant and temperature-resistant guar gum, such as Guojianchun and the like, under the alkali catalysis and the nitrogen protection, graft rigid pyrrolidone groups and ester groups onto a hydroxypropyl guar gum molecular chain to synthesize ultra-high temperature modified guar gum (Guojianchun and the like, research and application of the ultra-high temperature modified guar gum fracturing fluid, oilfield chemistry 2011, 28 (02): 201-205), and Wenella and the like modify hydroxypropyl guar gum by utilizing oleamidopropyl dimethyl tertiary amine to synthesize a novel high temperature-resistant hydroxypropyl guar gum with good hydrophobicity (such as Wenella and the like, the cross-linking rheological property of the high temperature-resistant guar gum fracturing fluid of the oleamidopropyl dimethyl tertiary amine modified hydroxypropyl guar gum with good hydrophobicity, oilfield chemistry 2020, 37 (04): 642-648), and Wenhui and the like, graft sulfonic acid groups onto the guar gum molecular chain, and the developed high temperature-resistant guar gum fracturing fluid can be researched and applied by using seawater preparation fluid (such as Bowenhui and the like, and the research and application of the high temperature-resistant guar gum fracturing fluid, and block breaking oil-gas fields, 2017, 24 (3): 434-436). Although the temperature resistance or salt tolerance of the guanidine gum is improved to a certain extent, the guanidine gum has the capability of not rapidly swelling in high-salinity brine within 5min, extra mixing equipment is needed, the salt tolerance of the amphoteric guanidine gum is greatly improved, and zwitterions are added, so that the preparation process is complex and the cost is high, and the temperature resistance and salt tolerance of the guanidine gum are not obviously improved.
Disclosure of Invention
The invention aims to provide a modified temperature-resistant salt-tolerant guanidine gum containing a conjugated group, which has excellent performance, overcomes the problems of slow swelling and dissolving speed, no high temperature resistance and no salt tolerance of the existing guanidine gum, and can meet the requirements of salt tolerance, high temperature resistance and continuous blending in large-scale fracturing construction in oil fields.
The invention also aims to provide a preparation method of the modified conjugate group-containing temperature-resistant salt-tolerant guanidine gum, which has the advantages of reliable principle and simple and convenient operation, improves the dissolution, salt tolerance and temperature tolerance of the guanidine gum by introducing a sulfonic acid group and a surfactant structure of a six-membered ring into the guanidine gum molecule, and has wide market application prospect.
In order to achieve the technical purpose, the invention adopts the following technical scheme.
The modified temperature-resistant salt-resistant guanidine gum containing the conjugated group has the following structural formula:
the preparation method of the modified temperature-resistant salt-resistant guanidine gum containing the conjugated group comprises the following steps:
SN reaction of aminoethanesulfonic acid with cyanuric chloride 2 Performing nucleophilic substitution reaction to obtain a chlorinated etherifying agent with surface activity, dissolving the chlorinated etherifying agent in an alcohol-water solvent to prepare a chlorinated etherifying agent solution, performing an alkalization reaction on the guar gum in the alcohol-water solvent, adding the chlorinated etherifying agent solution to perform an etherification reaction, and filtering, washing, neutralizing, drying, crushing and sieving the product to obtain the surfactant modified guar gum.
Further, the SN 2 Nucleophilic substitution reaction, wherein the molar ratio of the aminoethanesulfonic acid to the cyanuric chloride is 1-1.05, the solvent is acetone, the mass of the acetone is 70% of the total mass of reactants, the reaction is carried out for 5-6 h at the temperature of 0-5 ℃ and the pH value of 8-9 after feeding according to the proportion, the reaction solution is concentrated, cooled, filtered, washed and dried after the reaction is finished, and the chlorinated etherifying agent is obtained, and the structural formula is as follows:
further, in the preparation process of the chlorinated etherifying agent solution, the mass ratio of the chlorinated etherifying agent to the alcohol-water solvent is 20: and 80, adding the chlorinated etherifying agent into the alcohol-water solvent according to the proportion, and obtaining a chlorinated etherifying agent solution after magnetic stirring and full dissolution.
Further, the alkalization reaction is carried out by mixing guanidine gum: alcohol-water solvent: and (2) dispersing the guar gum in an alcohol-water solvent by using a 20% sodium hydroxide solution as a raw material according to a mass ratio of 33-41 to 54-63, and adding the 20% sodium hydroxide solution to perform an alkalization reaction for 30min to obtain an alkalized guar gum dispersion liquid.
Further, in the etherification reaction, the mass ratio of the chlorinated etherifying agent solution to the alkalized guar gum dispersion liquid is 17-30: 70-83, heating the alkalized guar gum dispersion liquid to 75 ℃, dropwise adding a chlorinated etherifying agent solution for 30min, and continuously reacting for 30min to obtain the surfactant modified guar gum, wherein the reaction process is as follows:
further, the alcohol-water solvent is ethanol, isopropanol or a mixture thereof, and the mass ratio of the alcohol to the water is 7-8.
In the washing process, the mass ratio of the aqueous solution of the alcohol to the modified guar gum is 3-4.
Further, in the neutralization process, the reagent is acetic acid, the mass of the acetic acid is 0.5-0.8% of the total mass of the reactants, and the acetic acid is added in the last washing process, and the pH = 6.5-7 is adjusted.
Further, in the drying, crushing and sieving processes, after drying for 24 hours in a thermostat with the temperature of 50 ℃, the mixture is taken out and crushed by a stirrer, and finally sieved by a vibrating sieve with 80 meshes to prepare the surfactant modified guanidine gum.
The reason why the guanidine gum can be dispersed in water is that hydroxyl on the molecular chain can form hydrogen bonds with water molecules, and the water molecules form a layer of water film around the molecular chain. In a high-concentration metal ion solution, metal ions are easy to attach to guanidine gum molecular chains through coordination with hydroxyl on the guanidine gum molecular chains, so that the action of the hydroxyl on the guanidine gum molecular chains and water molecules is blocked, and the guanidine gum molecular chains are limited from being dispersed in water. The sulfonate group on the modified guanidine gum molecular chain can be directionally complexed with metal ions in an aqueous solution, and the disordered accumulation and attachment of the metal ions on the guanidine gum molecular chain are avoided, so that the hydroxyl on the guanidine gum molecular chain can be exposed, and can be dispersed in water under the action of water, and the salt resistance of the guanidine gum is improved. Meanwhile, the guanidine gum molecular chain is grafted with an unsaturated cyclic structure, so that conjugated pi bonds can be formed among guanidine gum molecules, the action of the molecular chain is enhanced, and the spontaneous conjugated pi bonds can offset the reduction of the viscosity of the guanidine gum caused by the shearing action of part of the construction process, so that the modified guanidine gum has higher viscosity at high temperature and is suitable for high-temperature environments.
Compared with the prior art, the invention has the following beneficial effects:
the modified guanidine gum molecule contains sulfonic acid groups, and is easy to form a complex structure with metal ions, so that the influence on the swelling performance of the guanidine gum in saline water due to the action of main chain oxygen is avoided; unsaturated cyclic structures on the molecular chain form conjugated pi bonds, so that the acting force of the molecular chain is increased, and the salt resistance and temperature resistance of the guanidine gum are improved.
Specifically, the sulfonic acid group in the modified guanidine gum can effectively complex metal ions in the saline, prevent the metal ions from attaching to the surface of a guanidine gum molecular chain, inhibit the swelling of the guanidine gum and prevent effective acting force from being formed among the guanidine gum molecular chains. In water containing salt, particularly under the condition of containing calcium ions, the calcium ions can be complexed with four sulfonic acid groups, namely the salt for inhibiting the swelling of the guar gum is changed into the cross-linking ions capable of improving the viscosity performance of a guar gum system, and the viscosity of the guar gum can be effectively improved. In an aqueous solution, unsaturated cyclic structures on modified guanidine gum can increase intermolecular acting force through conjugated pi bonds to promote the guanidine gum to aggregate into a network structure, and molecules containing the conjugated structures can form the conjugated pi bonds as long as the distance between the molecules is in a proper range, so that the spontaneous bonds are formed in the shearing process to ensure enough intermolecular acting force in a guanidine gum system, thereby improving the temperature resistance of the guanidine gum system.
In conclusion, the invention starts from the structural principle and the principle of action with metal, and the guanidine gum is modified by the surfactant, so that the effects of salt resistance and temperature resistance can be fully exerted, the temperature resistance can reach 190 ℃, and the mineralization resistance can reach 8 ten thousand mg/L.
Drawings
FIG. 1 shows that the guar gum prepared in example 2 is prepared into 0.7% solution, 0.3% boron crosslinking agent is added, and 170s- 1 And shearing the rheological property test chart for 120 min.
FIG. 2 is a nuclear magnetic hydrogen spectrum of guar gum prepared in example 2.
Detailed Description
The invention is further illustrated below with reference to the figures and examples in order to facilitate the understanding of the invention by a person skilled in the art. It is to be understood that the invention is not limited in scope to the specific embodiments disclosed, but that various changes in form and detail will be suggested to one skilled in the art and are to be included within the spirit and purview of this application and scope of the appended claims.
Example 1
(1) Preparation of etherifying agent TCT-NS1
A250 ml four-necked flask was charged with 57.4g (65 wt%) of acetone, maintained at 0 ℃ in an ice bath, 18.4g (0.1 mol) of cyanuric chloride was added, stirred, and slowly added dropwise with 12.5g (0.1 mol) of aminoethanesulfonic acid solution, the pH being maintained at 8 with NaOH during the reaction. After the reaction is finished, concentrating, cooling and filtering the reaction liquid, washing the filter cake for 3 times by using acetone at the temperature of 0 ℃, and drying, crushing and sieving to obtain white powder, namely the etherifying agent TCT-NS1 with surface activity.
(2) Alkalization reaction
54g of guar gum is weighed and added into a three-neck flask, 91g of isopropanol and 13g of water are weighed and uniformly mixed and then added into the three-neck flask, stirring is started, the temperature is raised to 25 ℃, 6g of 20% sodium hydroxide solution is added, and alkalization is carried out for 30min.
(3) Etherification reaction
Weighing 7.2g of etherifying agent TCT-NS1, 25.2g of isopropanol and 3.6g of deionized water, uniformly stirring to obtain an etherifying agent TCT-NS1 solution, and adding the etherifying agent TCT-NS1 solution into a constant-pressure dropping funnel;
and after the alkalization reaction is finished, heating to 75 ℃, starting to dropwise add the etherifying agent TCT-NS1 solution for 30min, and continuing to react for 30min after the dropwise addition is finished.
(4) Post-treatment of modified guanidine gum
Carrying out suction filtration on the modified guanidine gum, then carrying out dispersion washing and suction filtration by using a solution consisting of isopropanol and water in a mass ratio of 4; in the third dispersion washing process, a neutralization reagent acetic acid is added for neutralization, and the pH of the system is =6.58; and after suction filtration, drying and crushing in a 50 ℃ drying oven to obtain the surfactant modified guar gum GG-TCT-NS.
Example 2
(1) Preparation of etherifying agent TCT-NS1
The same procedure as in example 1 was carried out to prepare a surface-active etherifying agent TCT-NS1.
(2) Alkalization reaction
54g of guar gum is weighed and added into a three-neck flask, 72.1g of absolute ethyl alcohol and 7.9g of water are weighed and uniformly mixed, then the mixture is added into the three-neck flask, stirring is started, the temperature is raised to 25 ℃, 6g of 20% sodium hydroxide solution is added, and alkalization is carried out for 30min.
(3) Etherification reaction
Weighing 9.2g of etherifying agent TCT-NS1, 16g of isopropanol, 16.2g of absolute ethyl alcohol and 4.6g of deionized water, uniformly stirring to obtain an etherifying agent TCT-NS1 solution, and adding the etherifying agent TCT-NS1 solution into a constant-pressure dropping funnel;
and after the alkalization reaction is finished, heating to 75 ℃, starting to dropwise add the etherifying agent TCT-NS1 solution for 30min, and continuing to react for 30min after the dropwise addition is finished.
(4) Post-treatment of modified guanidine gum
Carrying out suction filtration on the modified guanidine gum, then carrying out dispersion washing and suction filtration by using a solution consisting of isopropanol and water in a mass ratio of 4; in the third dispersing and washing process, adding a neutralizing agent acetic acid for neutralization, wherein the pH of the system is =6.88; and after suction filtration, drying and crushing in a 50 ℃ drying oven to obtain the surfactant modified guar gum GG-TCT-NS.
Example 3
(1) Preparation of etherifying agent TCT-NS1
The same procedure as in example 1 was carried out to prepare a surface-active etherifying agent TCT-NS1.
(2) Alkalization reaction
54g of guanidine gum is weighed and added into a three-neck flask, 80.5g of isopropanol and 11.5g of water are weighed and uniformly mixed, then the mixture is added into the three-neck flask, stirring is started, the temperature is raised to 25 ℃, 8g of 20% sodium hydroxide solution is added, and alkalization is carried out for 30min.
(3) Etherification reaction
Weighing 12.4g of etherifying agent TCT-NS1, 43.4g of isopropanol and 6.2g of deionized water, uniformly stirring to obtain an etherifying agent TCT-NS1 solution, and adding the solution into a constant-pressure dropping funnel;
and after the alkalization reaction is finished, heating to 75 ℃, starting to dropwise add the etherifying agent TCT-NS1 solution for 30min, and continuing to react for 30min after the dropwise addition is finished.
(4) Post-treatment of modified guanidine gum
Carrying out suction filtration on the modified guanidine gum, then carrying out dispersion washing and suction filtration by using a solution consisting of isopropanol and water in a mass ratio of 3; in the third dispersing and washing process, adding a neutralizing agent acetic acid for neutralization, wherein the pH of the system is =6.58; and after suction filtration, drying and crushing in a 50 ℃ drying oven to obtain the surfactant modified guar gum GG-TCT-NS.
Example 4
(1) Preparation of etherifying agent TCT-NS2
57.4g (65 wt%) of acetone were added to a 250ml four-necked flask, the temperature was maintained at 5 ℃ in an ice bath, 18.4g (0.1 mol) of cyanuric chloride was added, stirred, and 13.1g (0.15 mol) of aminoethanesulfonic acid solution was slowly added dropwise, and the pH was maintained at 9 during the reaction with NaOH. After the reaction is finished, concentrating, cooling and filtering the reaction solution, washing the filter cake for 5 times by using acetone at the temperature of 5 ℃, and drying, crushing and sieving to obtain the white powder etherifying agent TCT-NS2 with surface activity.
(2) Alkalization reaction
54g of guar gum is weighed and added into a three-neck flask, 80.5g of isopropanol and 11.5g of water are weighed and uniformly mixed and then added into the three-neck flask, stirring is started, the temperature is raised to 25 ℃, 4g of 20% sodium hydroxide solution is added, and alkalization is carried out for 30min.
(3) Etherification reaction
Weighing 6g of etherifying agent TCT-NS2, 21g of isopropanol and 3g of deionized water, uniformly stirring to obtain an etherifying agent TCT-NS2 solution, and adding the etherifying agent TCT-NS2 solution into a constant-pressure dropping funnel;
and after the alkalization reaction is finished, heating to 75 ℃, starting to dropwise add the etherifying agent TCT-NS2 solution for 30min, and continuing to react for 30min after the dropwise addition is finished.
(4) Post-treatment of modified guar gum
Carrying out suction filtration on the modified guanidine gum, then carrying out dispersion washing and suction filtration by using a solution consisting of isopropanol and water in a mass ratio of 4; in the third dispersing and washing process, adding a neutralizing agent acetic acid for neutralization, wherein the pH of the system is =6.68; and after suction filtration, drying and crushing in a 50 ℃ drying oven to obtain the surfactant modified guar gum GG-TCT-NS.
Example 5
(1) Preparation of etherifying agent TCT-NS2
The same procedure as in example 4 was used to prepare a surface-active etherifying agent TCT-NS2.
(2) Alkalization reaction
54g of guar gum is weighed and added into a three-neck flask, 42g of ethanol and 6g of water are weighed and uniformly mixed, then the mixture is added into the three-neck flask, stirring is started, the temperature is raised to 25 ℃, 6g of 20% sodium hydroxide solution is added, and alkalization is carried out for 30min.
(3) Etherification reaction
Weighing 9.2g of etherifying agent TCT-NS2, 20g of isopropanol, 12.7g of absolute ethyl alcohol and 4.1g of deionized water, uniformly stirring to obtain an etherifying agent TCT-NS2 solution, and adding the etherifying agent TCT-NS2 solution into a constant-pressure dropping funnel;
and after the alkalization reaction is finished, heating to 75 ℃, starting to dropwise add the etherifying agent TCT-NS2 solution for 30min, and continuing to react for 30min after the dropwise addition is finished.
(4) Post-treatment of modified guanidine gum
Carrying out suction filtration on the modified guanidine gum, then carrying out dispersion washing and suction filtration by using a solution consisting of isopropanol and water with the mass ratio of 3.5; in the third dispersing and washing process, adding a neutralizing agent acetic acid for neutralization, wherein the pH of the system is =7; and after suction filtration, drying and crushing in a 50 ℃ drying oven to obtain the surfactant modified guar gum GG-TCT-NS.
Comparative example
54g of guar gum is weighed and added into a three-neck flask, 91g of isopropanol and 13g of water are weighed and uniformly mixed and then added into the three-neck flask, stirring is started, the temperature is raised to 25 ℃, 4g of 20% sodium hydroxide solution is added, and alkalization is carried out for 30min.
21g of isopropanol and 9g of deionized water are uniformly stirred to obtain an alcohol-water solution, and the alcohol-water solution is added into a constant-pressure dropping funnel;
and after the alkalization reaction is finished, heating to 75 ℃, beginning to dropwise add the alcohol-water solution for 30min, and continuing to react for 30min after the dropwise addition is finished.
Carrying out suction filtration on the guanidine gum after reaction, then carrying out dispersion washing and suction filtration by using a solution consisting of isopropanol and water with the mass ratio of 4; in the third dispersing and washing process, adding a neutralizing agent acetic acid for neutralization, wherein the pH of the system is =7; and after suction filtration, drying in a 50 ℃ oven, and crushing to obtain the guanidine gum of the comparative example without etherification reaction.
The guar gums prepared according to examples 1-5 and comparative examples were prepared as 0.6% solutions and tested for apparent viscosity at different times using a six-speed viscometer, the results of which are shown in table 1.
As can be seen from Table 1, the guar gum modified by the chlorinated etherifying agent has a dissolution rate equivalent to that of the guar gum modified by the chlorinated etherifying agent (with low molecular weight) and a high dissolution rate, but the apparent viscosity of the guar gum modified by the chlorinated etherifying agent is much higher than that of the guar gum without the chlorinated etherifying agent in the same time.
TABLE 1 dissolution thickening Performance of guar gums of the different examples
The modified guar gum prepared in example 2 was formulated into a 0.7% solution and tested for rheological properties by adding 0.3% boron crosslinker (see figure 1). As can be seen from the figure, the apparent viscosity is 70mPa.s at 190 ℃ and under shearing at 170s < -1 > for 120 min.
The molecular functional group structure of the synthesized sample was further examined using nuclear magnetic hydrogen spectroscopy using the modified guar gum prepared in example 2 (see fig. 2). As can be seen from fig. 2, the nmr spectrum showed that oxygen atoms were present in the vicinity of hydrogen on the synthesized guar branches, so that the peak of hydrogen atoms directly linked to carbon was mainly present between 3.5 and 4.2ppm, and the peak position not linked to carbon but linked to hydrogen and oxygen was present between 4.7 and 4.9ppm, thus confirming that the modified guar thickener was the target product.
Claims (10)
1. The modified temperature-resistant salt-resistant guanidine gum containing the conjugated group has the following structural formula:
2. the preparation method of the modified conjugate group-containing temperature-resistant salt-tolerant guanidine gum as claimed in claim 1, which comprises the following steps:
SN reaction of aminoethanesulfonic acid with cyanuric chloride 2 Nucleophilic substitution reaction to obtain a chlorinated etherifying agent with surface activity, dissolving the chlorinated etherifying agent in an alcohol-water solvent to prepare a chlorinated etherifying agent solution, carrying out an alkalization reaction on the guar gum in the alcohol-water solvent, adding the chlorinated etherifying agent solution to carry out an etherification reaction, and filtering, washing, neutralizing, drying, crushing and sieving the product to obtain the surfactant modified guar gum.
3. Such as the rightThe method of claim 2, wherein the SN is 2 And (2) nucleophilic substitution reaction, wherein the molar ratio of the aminoethanesulfonic acid to the cyanuric chloride is 1-1.05, the solvent is acetone, the mass of the acetone is 70% of the total mass of the reactants, the reaction is carried out for 5-6 h at the temperature of 0-5 ℃ and the pH value of 8-9 after feeding according to the proportion, and the reaction solution is concentrated, cooled, filtered, washed and dried after the reaction is finished, so that the chlorinated etherifying agent is obtained.
4. The method according to claim 2, wherein in the preparation process of the solution of the chlorinated etherifying agent, the mass ratio of the chlorinated etherifying agent to the alcohol-water solvent is 20: and 80, adding the chlorinated etherifying agent into the alcohol-water solvent according to the proportion, and obtaining a chlorinated etherifying agent solution after magnetic stirring and full dissolution.
5. The method of claim 2, wherein the alkalization reaction is performed in the presence of a guanidine gum: alcohol-water solvent: and (2) dispersing the guar gum in an alcohol-water solvent by using a 20% sodium hydroxide solution as a raw material according to a mass ratio of 33-41 to 54-63, and adding the 20% sodium hydroxide solution to perform an alkalization reaction for 30min to obtain an alkalized guar gum dispersion liquid.
6. The method according to claim 2, wherein the mass ratio of the chlorinated etherifying agent solution to the alkalized guar gum dispersion in the etherification reaction is 17-30: 70-83, heating the alkalized guar gum dispersion liquid to 75 ℃, dropwise adding a chlorinated etherifying agent solution for 30min, and continuously reacting for 30min to obtain the surfactant modified guar gum.
7. The method according to claim 2, 4 or 5, wherein the alcohol-water solvent is ethanol, isopropanol or a mixture thereof, and the mass ratio of the alcohol to the water is 7-8.
8. The method according to claim 2, wherein in the washing process, the mass ratio of the aqueous alcohol solution to the modified guar gum is 3-4.
9. The method of claim 2, wherein the neutralization process, the reagent is acetic acid, the mass of acetic acid is 0.5-0.8% of the total mass of reactants, and the pH is adjusted to be 6.5-7 during the last washing.
10. The method of claim 2, wherein the drying, crushing and sieving processes comprise drying in a thermostat at 50 ℃ for 24 hours, taking out, crushing by a stirrer, and finally sieving by a vibrating sieve of 80 meshes to obtain the surfactant modified guanidine gum.
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2022
- 2022-09-19 CN CN202211139744.2A patent/CN115466337A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 赵素粉等: "阴离子瓜尔胶的制备及其稀溶液性质", 天津化工 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116063585A (en) * | 2023-02-27 | 2023-05-05 | 中海油田服务股份有限公司 | Modified temperature-resistant guanidine gum and preparation method thereof |
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