CN112724050A - Phosphorus-free alkali-resistant solubilizer and preparation and application thereof - Google Patents

Phosphorus-free alkali-resistant solubilizer and preparation and application thereof Download PDF

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CN112724050A
CN112724050A CN202011605577.7A CN202011605577A CN112724050A CN 112724050 A CN112724050 A CN 112724050A CN 202011605577 A CN202011605577 A CN 202011605577A CN 112724050 A CN112724050 A CN 112724050A
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resistant
solubilizer
fatty alcohol
free alkali
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CN112724050B (en
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付艳梅
李东旭
程玄
潘琦
黄开伟
李正华
耿聪
江晨浩
张静
王亮
王辉
任凡
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Wuhan Oxiran Specialty Chemicals Co
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    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/32Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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    • C07C309/00Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/01Sulfonic acids
    • C07C309/02Sulfonic acids having sulfo groups bound to acyclic carbon atoms
    • C07C309/03Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
    • C07C309/07Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing oxygen atoms bound to the carbon skeleton
    • C07C309/09Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing oxygen atoms bound to the carbon skeleton containing etherified hydroxy groups bound to the carbon skeleton
    • C07C309/10Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing oxygen atoms bound to the carbon skeleton containing etherified hydroxy groups bound to the carbon skeleton with the oxygen atom of at least one of the etherified hydroxy groups further bound to an acyclic carbon atom
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    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
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Abstract

The invention provides a phosphorus-free alkali-resistant solubilizer which is an aqueous solution of fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) sulfonate, wherein the structural general formula of the fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) sulfonate is as follows:
Figure DDA0002873244750000011
wherein m is 2-10 and n is 1-5. The solubilizer is synthesized by fatty alcohol/alkylphenol polyoxyethylene/propylene ether and 1, 3-propane sultone. The solubilizer is phosphorus-free, meets the national first-level emission standard, has stable structure and hasGood temperature resistance and weather resistance, and no change of the performance over the years; has good solubility, can replace phosphate solubilizer and has good saline-alkali resistance.

Description

Phosphorus-free alkali-resistant solubilizer and preparation and application thereof
Technical Field
The invention relates to a functional special surfactant, in particular to an alkali-resistant solubilizer, and particularly relates to a phosphorus-free surfactant with alkali-resistant solubilization effect.
Background
In recent years, people have stronger environmental awareness along with more and more strict national environmental control. The industrial cleaning sewage needs to be treated in a complex way to meet the environmental protection requirements of low COD and low VOC. The surfactants and the associated solubilizers used must therefore meet environmental requirements.
The solubilizers available on the market can be roughly divided into several classes. The first, phenoxy phosphates, as in patent applications PCT/CN2014/077114, US8,147,681B2, etc. The second class, alkylglycoside structures, such as those described in patent applications CN108949394A, CN110270269A, and the like. The third class, amino ester salt structures, is described in patent applications WO2015/155095, WO2020/1535200, and the like. The fourth class, sulfonic acid/carboxylate structures, as in patent applications CN108618991A, JP-349441/2002, and the like. These solubilizers having different structures have problems in practical use. Wherein, the use of the phosphate has the problem of overproof phosphorus content; the stability problem of the amino ester and the sulfonic acid/carboxylate in severe environment is solved; alkyl glycoside solubilizers are generally relatively expensive and have limited solubilizing effect in high-concentration alkaline (salt) solutions.
Therefore, a phosphorus-free alkali-resistant solubilizer which overcomes the defects is needed to meet more severe industrial and environmental requirements.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide a phosphorus-free alkali-resistant solubilizer which has good alkali resistance and solubilization.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
in a first aspect, an embodiment of the present invention provides a phosphorus-free alkali-resistant solubilizer, where the phosphorus-free alkali-resistant solubilizer is an aqueous solution of fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) allylether sulfonate, and a structural general formula of the fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) allylether sulfonate is as follows:
Figure BDA0002873244730000021
wherein m is 2-10 and n is 1-5.
In a second aspect, an embodiment of the present invention provides a method for preparing the phosphorus-free alkali-resistant solubilizing agent, which includes the following steps:
firstly, carrying out high-speed stirring sulfonation reaction on fatty alcohol/alkylphenol polyoxyethylene/propylene ether and a certain amount of 1.3-propane sultone under the conditions of 80-100 ℃ and 90-101 kpa of negative pressure for 2.5-3.5 hours to obtain a reaction solution;
step two, cooling the reaction liquid prepared in the step one to 20-25 ℃, adding an extraction liquid for extraction and purification, and removing salt which is not reacted completely;
and step three, removing the extract mixed liquor of the residues in the step two, distilling the extract mixed liquor by using a rotary evaporator to remove the solvent, and adjusting the solid content of the obtained product to 65-85% by using deionized water to obtain the phosphorus-free alkali-resistant solubilizer.
In a third aspect, the embodiments of the present invention provide an application of the above phosphorus-free alkali-resistant solubilizing agent, where the phosphorus-free alkali-resistant solubilizing agent is applied to a saline solution or an alkaline solution to solubilize a nonionic surfactant.
Compared with the prior art, the phosphorus-free alkali-resistant solubilizer is an aqueous solution of potassium/ammonium salt of fatty alcohol/alkylphenol polyoxyethylene/propylene ether sulfonic acid, has good alkali-resistant solubilization and excellent solubilization effects, particularly has good solubilization effect on a nonionic surfactant in a complex environment, enables the surfactant to be uniformly dispersed in the solution, ensures the directional functionality of the solution, and has long-term stability; in the cleaning process, the harsh environment resistance is good; in addition, the phosphorus-free alkali-resistant solubilizer does not contain phosphorus, thereby effectively reducing the environmental pollution caused by the discharge of chemical oxygen demand.
Drawings
FIG. 1 is the nuclear magnetic structure map of the alkali-resistant solubilizing agent obtained in example 1 and example 4 of the present invention, wherein FIG. (A) is the nuclear magnetic structure map of the alkali-resistant solubilizing agent obtained in example 1, and FIG. (B) is the nuclear magnetic structure map of the alkali-resistant solubilizing agent obtained in example 4.
FIG. 2 is a graph showing the solubilizing ability of the solubilizing agent obtained in example 2 for high foam surfactant (OP-10)/low foam surfactant (DP-106) in a base/salt solution formulation; wherein (a) and (b) are respectively the state before the high foaming surfactant (OP-10) and the low foaming surfactant (DP-106) (in the system of Table 1) are added with the solubilizer, and (c) and (d) are the state after the high foaming surfactant (OP-10) and the low foaming surfactant (EP-61) are added with the solubilizer.
Detailed Description
Embodiments of the present invention will be described in detail below. The embodiments of the invention should not be construed as limiting the invention.
The embodiment of the invention provides a phosphorus-free alkali-resistant solubilizer which can solubilize a nonionic surfactant in an alkali (salt) complex environment and has long-term stability. The phosphorus-free alkali-resistant solubilizer is an aqueous solution of fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) sulfonate, and the structural general formula of the fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) sulfonate is as follows:
Figure BDA0002873244730000031
wherein m is 2-10 and n is 1-5.
In some embodiments, the sodium (potassium) fatty alcohol/alkylphenol polyoxyethylene/propylene ether sulfonate salt comprises at least one of a sodium fatty alcohol polyoxyethylene/propylene ether sulfonate salt, a potassium fatty alcohol polyoxyethylene/propylene ether sulfonate salt, a sodium alkylphenol polyoxyethylene/propylene ether sulfonate salt, and a potassium alkylphenol polyoxyethylene/propylene ether sulfonate salt.
The embodiment of the invention also provides a preparation method of the phosphorus-free alkali-resistant solubilizer, which comprises the following steps:
firstly, carrying out high-speed stirring sulfonation reaction on fatty alcohol/alkylphenol polyoxyethylene/propylene ether and a certain amount of 1.3-propane sultone under the conditions of 80-100 ℃ and 90-101 kpa of negative pressure for 2.5-3.5 hours to obtain a reaction solution;
step two, cooling the reaction liquid prepared in the step one to 20-25 ℃, adding an extraction liquid for extraction and purification, and removing salt which is not reacted completely;
and step three, distilling the extract mixed liquor with residues removed in the step two by using a rotary evaporator to remove the solvent, and adjusting the solid content of a product obtained after the solvent is removed to 65-85% by using deionized water to obtain the phosphorus-free alkali-resistant solubilizer.
In the fatty alcohol/alkylphenol polyoxyethylene/propylene ether, the fatty alcohol may be, but is not limited to, an eight-to eighteen-carbon isomer fatty alcohol. In some embodiments, the fatty alcohol comprises at least one of isooctanol, isononanol, isomeric decanols, isomeric undecanols, isomeric tridecanols, and isomeric hexadecanoyl-octadecanols, and the alkyl phenol comprises at least one of nonyl phenol, octyl phenol, m-cresol, t-butyl phenol, 2-naphthol, and p-cumyl phenol.
In the fatty alcohol/alkylphenol polyoxyethylene/propylene ether, the polyoxypropylene can be but is not limited to propylene oxide, and the addition number n is 1-5.
In the fatty alcohol/alkylphenol polyoxyethylene/propylene ether, the polyoxyethylene can be but is not limited to ethylene oxide addition number m of 2-10.
In some embodiments, in the first step, the alkaline environment is an alkaline environment mixture formed by mixing a base including at least one of potassium hydroxide, sodium hydroxide, potassium tert-butoxide, sodium tert-butoxide, potassium methoxide, sodium hydride, and potassium hydride with the fatty alcohol/alkylphenol polyoxyethylene/propylene ether under high-speed stirring at 120-150 ℃. Optionally, the stirring speed is 500-600 r/min.
In some embodiments, the base is used in a molar fraction of 1.5 to 2.5 times that of the fatty alcohol/alkylphenol polyoxyethylene/propylene ether.
In some embodiments, the molar ratio of the fatty alcohol/alkylphenol polyoxyethylene/propylene ether to the 1.3-propane sultone is 1:1.25 to 2.25.
In some embodiments, in the step one, the stirring speed during the sulfonation reaction is 500 to 600 r/min.
In some embodiments, in step two, the extract comprises at least one of n.n-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), Dimethylacetamide (DMAC), ethyl acetate, N-methylpyrrolidone (NMP), and dimethyl ether (DME).
The embodiment of the invention also provides application of the phosphorus-free alkali-resistant solubilizer, which is applied to a salt solution or an alkali solution to solubilize a nonionic surfactant.
In some embodiments, the amount of the phosphorus-free alkali-resistant solubilizer is 0.5 to 1.5 times that of the nonionic surfactant.
In some embodiments, the phosphorus-free alkali-resistant solubilizer is used at a temperature of-15 to 60 ℃.
In some embodiments, the salt solution has a concentration of 5-25%, and the salt in the salt solution comprises (meta) sodium silicate, sodium citrate, borate, chromate, manganate.
In some embodiments, the concentration of the alkali solution is 5-25%, and the alkali in the alkali solution comprises KOH, NaOH and Na2CO3
The phosphorus-free alkali-resistant solubilizer is an aqueous solution of potassium/ammonium salt of fatty alcohol/alkylphenol polyoxyethylene/propylene ether sulfonic acid, has good alkali-resistant solubilization and excellent solubilization effects, particularly has good solubilization effect on a nonionic surfactant in a complex environment, enables the surfactant to be uniformly dispersed in the solution, ensures the directional functionality of the solution, and has long-term stability; in the cleaning process, the harsh environment resistance is good; in addition, the phosphorus-free alkali-resistant solubilizer does not contain phosphorus, thereby effectively reducing the environmental pollution caused by the discharge of chemical oxygen demand.
The preparation method and performance of the phosphorus-free alkali-resistant solubilizing agent of the present invention will be described below with reference to specific examples.
Example 1
To a 1L three necked round bottom flask equipped with a thermometer and mechanical stirrer and connected to a nitrogen inlet tube was added 1.00 equivalents (i.e., 1mol) of a fatty alcohol polyoxyethylene/propylene ether, 1.50 equivalents of a base (0.75 equivalents each of potassium methoxide and potassium hydroxide). And then starting mechanical stirring (rotating speed is 500-600 r/min) in an oil bath kettle with a temperature control system, introducing nitrogen to the bottom of the flask, controlling the flow rate (2 bubbles/second on the liquid surface, paying attention to evacuation), introducing the nitrogen for 30min, and then starting heating reaction at the reaction temperature of 120-150 ℃. The reaction time is 5-7 hours, and the process is continuously protected by nitrogen. The first stage reaction is completed, the product is brown viscous liquid, and the introduction of nitrogen is stopped.
Cooling to 80-100 ℃, starting vacuum, degassing until no material expansion bubbles exist in the system or material expansion is stable, starting constant-pressure dropping of 1.3-propane sultone with the temperature kept at 50 ℃, starting a vacuum pump in the whole process, controlling the vacuum degree at 90-101 KPa, and controlling the dropping time within 10 min. Then, the reaction is carried out for 2-3 hours under heat preservation, and the whole stirring process is maintained at 500-600 r/min. After the reaction was complete, a reddish brown viscous liquid was obtained.
Then, cooling to below 60 ℃, adding N, N-Dimethylformamide (DMF) with the mass of 1.5 times of that of the total product, fully stirring, standing for 3-5h, extracting and separating, and then distilling by a rotary evaporator to remove the organic solvent. Finally, water is added to adjust the solid content to 65% -85%, and the final product is obtained and is marked as solubilizer A.
FIG. 1 (A) is a nuclear magnetic structural map of the final product obtained in example 1. As can be seen from FIG. 1, the main component of the final product obtained in example 1 was the potassium salt of fatty alcohol-polyoxyethylene/propylene ether sulfonate. Five groups of peaks in the nuclear magnetic structural map shown in (a) in fig. 1 respectively reflect the response forms of three forms of protons H, and the structural general formula is:
Figure BDA0002873244730000061
wherein a is 8-18, m is 1-10, and n is 8-18.
Example 2
To a 1L three necked round bottom flask equipped with a thermometer and mechanical stirrer and connected to a nitrogen inlet tube was added 1.00 equivalents (i.e. 1mol) of fatty alcohol polyoxyethylene/propylene ether, 2.14 equivalents of base (1.07 equivalents each of sodium hydride and sodium hydroxide). And then starting mechanical stirring (rotating speed is 500-600 r/min) in an oil bath kettle with a temperature control system, introducing nitrogen to the bottom of the flask, controlling the flow rate (2 bubbles/second on the liquid surface, paying attention to evacuation), introducing the nitrogen for 30min, and then starting heating reaction at the reaction temperature of 120-150 ℃. The reaction time is 5-7 hours, and the process is continuously protected by nitrogen. The first stage reaction is completed, the product is brown viscous liquid, and the introduction of nitrogen is stopped.
Cooling to 80-100 ℃, starting vacuum, degassing until no material expansion bubbles exist in the system or material expansion is stable, starting constant-pressure dropping of 1.3-propane sultone with the temperature kept at 50 ℃, starting a vacuum pump in the whole process, controlling the vacuum degree at 90-101 KPa, and controlling the dropping time within 10 min. Then, the reaction is carried out for 2-3 hours under heat preservation, and the whole stirring process is maintained at 500-600 r/min. After the reaction was complete, a reddish brown viscous liquid was obtained.
And then, cooling to below 60 ℃, adding Dimethylacetamide (DMAC) with the same mass as the total product, fully stirring, standing for 3-5h, extracting and separating, and distilling by a rotary evaporator to remove the organic solvent. Finally, water is added to adjust the solid content to 65% -85%, and the final product is obtained and is marked as solubilizer B. The final product is a water solution of fatty alcohol polyoxyethylene/propylene ether sulfonic acid sodium salt, and the structural general formula of the fatty alcohol polyoxyethylene/propylene ether sulfonic acid sodium salt is as follows:
Figure BDA0002873244730000062
wherein a is 8-18, m is 1-10, and n is 8-18.
Example 3
To a 1L three necked round bottom flask equipped with a thermometer and mechanical stirrer and connected to a nitrogen inlet line was added 1.00 equivalents (i.e., 1mol) of alkylphenol polyoxyethylene/propylene ether, 1.15 equivalents of sodium tert-butoxide. Starting mechanical stirring (rotating speed is 500-600 r/min) in an oil bath pan with a temperature control system, introducing nitrogen to the bottom of a flask, controlling the flow rate (2 bubbles/second on the liquid surface, paying attention to evacuation), introducing nitrogen for 30min, and then starting heating reaction at the reaction temperature of 120-150 ℃. The reaction time is 5-7 hours, and the process is continuously protected by nitrogen. The first stage reaction is completed, the product is brown viscous liquid, and the introduction of nitrogen is stopped.
Cooling to 80-100 ℃, starting vacuum, degassing until no material expansion bubbles exist in the system or material expansion is stable, starting constant-pressure dropping of 1.3-propane sultone with the temperature kept at 50 ℃, starting a vacuum pump in the whole process, controlling the vacuum degree at 90-101 KPa, and controlling the dropping time within 10 min. Then, the reaction is carried out for 2-3 hours under heat preservation, and the whole stirring process is maintained at 500-600 r/min. After the reaction was complete, a reddish brown viscous liquid was obtained.
And then, cooling to below 60 ℃, adding ethyl acetate with the mass of 1.2 times of that of the total product, fully stirring, standing for 3-5h, extracting and separating, and distilling by a rotary evaporator to remove the organic solvent. Finally, water is added to adjust the solid content to 65% -85%, and the final product is obtained and is marked as solubilizer C. The final product is an aqueous solution of sodium alkylphenol polyoxyethylene/propylene ether sulfonate, and the structural general formula of the sodium alkylphenol polyoxyethylene/propylene ether sulfonate is as follows:
Figure BDA0002873244730000071
wherein m is 1-10, and n is 8-18.
Example 4
To a 1L three necked round bottom flask equipped with a thermometer and mechanical stirrer and connected to a nitrogen inlet tube was added 1.00 equivalents (i.e., 1mol) of alkylphenol polyoxyethylene/propylene ether, 2.50 equivalents of base (1.50 equivalents of potassium hydride and 1.00 equivalents of potassium hydroxide). And then starting mechanical stirring (rotating speed is 500-600 r/min) in an oil bath kettle with a temperature control system, introducing nitrogen to the bottom of the flask, controlling the flow rate (2 bubbles/second on the liquid surface, paying attention to evacuation), introducing the nitrogen for 30min, and then starting heating reaction at the reaction temperature of 120-150 ℃. The reaction time is 5-7 hours, and the process is continuously protected by nitrogen. The first stage reaction is completed, the product is brown viscous liquid, and the introduction of nitrogen is stopped.
Cooling to 80-100 ℃, starting vacuum, degassing until no material expansion bubbles exist in the system or material expansion is stable, starting constant-pressure dropping of 1.3-propane sultone with the temperature kept at 50 ℃, starting a vacuum pump in the whole process, controlling the vacuum degree at 90-101 KPa, and controlling the dropping time within 10 min. Then, the reaction is carried out for 2-3 hours under heat preservation, and the whole stirring process is maintained at 500-600 r/min. After the reaction was complete, a reddish brown viscous liquid was obtained.
Then, cooling to below 60 ℃, adding dimethyl ether (DME) with the mass 1.4 times of that of the total product, fully stirring, standing for 3-5h, extracting and separating, and distilling by a rotary evaporator to remove the organic solvent. Finally, water is added to adjust the solid content to 65% -85%, and the final product is obtained and is marked as solubilizer D.
FIG. 1 (B) is a nuclear magnetic structural map of the final product obtained in example 4. As can be seen from fig. 1, the main component of the final product obtained in example 4 was potassium salt of alkylphenol polyoxyethylene/propylene ether sulfonate. Five groups of peaks in the nuclear magnetic structural map shown in (B) in fig. 1 respectively reflect the response forms of three forms of protons H, and the structural general formula is:
Figure BDA0002873244730000081
wherein m is 1-10, and n is 8-18.
The solubilizing agent A, B, C, D obtained in examples 1-4 was tested for alkali/salt solubility enhancement using the solubilizing system described in Table 1. The test performance is shown in Table 2.
TABLE 1 solubilization System composition
Solubilizing system component Solid content (mass percentage)
High foaming surfactant (OP-10)/Low foaming surfactant (DP-106) 5%
Sodium metasilicate pentahydrate 5%
Sodium hydroxide 5%
Solubilizer To be measured
Water (W) Balance of
TABLE 2 basic Performance comparison Table of solubilizers A/B/C/D
Figure BDA0002873244730000082
Wherein, when testing static/dynamic surface tension, the solubilizer A, B, C, D is prepared into 1g/L aqueous solution respectively. The solubilizing amount is the compatibilization amount after uniformly converting 50% of solid content, for example, taking the solubilizing agent A as an example, the amount of the 75.32% solid content solubilizing high-foaming surfactant is 2.66%, and the calculation process of the amount of the 50% solid content solubilizing high-foaming surfactant is as follows: 2.66% ÷ [1- (75.32% -50%) ] -3.56%, (test temperature 20 ℃).
FIG. 2 shows the solubilizing power of the solubilizing agent obtained in example 2 of the present invention for high foam surfactant (OP-10)/low foam surfactant (DP-106) in the formulation of alkali/salt solution. Wherein (a) and (b) are respectively the states before the high foaming surfactant (OP-10) and the low foaming surfactant (DP-106) (in the system of Table 1) are added with the solubilizer; (c) and (d) is the state of the high foaming surfactant (OP-10) and the low foaming surfactant (EP-61) (in the system of Table 1) after addition of the solubilizer. As can be seen from FIG. 2, the solution is clear and transparent after the solubilizer is added, and the solubilizer has excellent solubilizing effect.
The raw materials listed in the invention, the values of the upper limit and the lower limit and the interval of the raw materials, and the values of the upper limit and the lower limit and the interval of the process parameters can all realize the invention, and the examples are not listed.
In addition, other changes may be made by those skilled in the art within the spirit of the application, and such changes are, of course, encompassed within the scope of the invention as claimed.

Claims (10)

1. The phosphorus-free alkali-resistant solubilizer is characterized in that the phosphorus-free alkali-resistant solubilizer is an aqueous solution of fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) sulfonate, and the structural general formula of the fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) sulfonate is as follows:
Figure FDA0002873244720000011
wherein m is 2-10 and n is 1-5.
2. The phosphorus-free alkali-resistant solubilizing agent of claim 1, wherein the fatty alcohol/alkylphenol polyoxyethylene/sodium (potassium) sulfonate comprises at least one of fatty alcohol polyoxyethylene/propylene ether sulfonate sodium salt, fatty alcohol polyoxyethylene/propylene ether sulfonate potassium salt, alkylphenol polyoxyethylene/propylene ether sulfonate sodium salt and alkylphenol polyoxyethylene/propylene ether sulfonate potassium salt.
3. A process for preparing the phosphorus-free alkali-resistant solubilizing agent according to claim 1 or 2, comprising the steps of:
firstly, carrying out high-speed stirring sulfonation reaction on fatty alcohol/alkylphenol polyoxyethylene/propylene ether and a certain amount of 1.3-propane sultone under the conditions of 80-100 ℃ and 90-101 kpa of negative pressure for 2.5-3.5 hours to obtain a reaction solution;
step two, cooling the reaction liquid prepared in the step one to 20-25 ℃, adding an extraction liquid for extraction and purification, and removing salt which is not reacted completely;
and step three, distilling the extract mixed liquor with residues removed in the step two by using a rotary evaporator to remove the solvent, and adjusting the solid content of a product obtained after the solvent is removed to 65-85% by using deionized water to obtain the phosphorus-free alkali-resistant solubilizer.
4. The method of claim 3, wherein said aliphatic alcohol/alkylphenol polyoxyethylene/allyl ether comprises at least one of isooctanol, isononanol, isomeric decanol, isomeric undecanol, isomeric tridecanol and isomeric hexadecadecanol, said alkylphenol comprises at least one of nonylphenol, octylphenol, m-cresol, tert-butylphenol, 2-naphthol and cumylphenol, said polyoxypropylene is propylene oxide adduct number n is 1-5, and said polyoxyethylene is ethylene oxide adduct number m is 2-10.
5. The method of claim 3, wherein in step one, the alkaline environment is a mixture of at least one of potassium hydroxide, sodium hydroxide, potassium tert-butoxide, sodium tert-butoxide, potassium methoxide, sodium hydride and potassium hydride and the fatty alcohol/alkylphenol polyoxyethylene/propenyl ether under high speed stirring at 120-150 ℃.
6. The method for preparing phosphorus-free alkali-resistant solubilizer according to claim 3, wherein the molar ratio of the fatty alcohol/alkylphenol polyoxyethylene/propylene ether to the 1.3-propane sultone is 1: 1.25-2.25.
7. The method of claim 3, wherein the extraction liquid comprises at least one of N, N-dimethylformamide, dimethyl sulfoxide, dimethylacetamide, ethyl acetate, N-methylpyrrolidone, and dimethyl ether.
8. The use of the phosphorus-free alkali-resistant solubilizer according to claim 1 or 2, wherein the phosphorus-free alkali-resistant solubilizer is used in a salt solution or an alkali solution to solubilize the nonionic surfactant, and the dosage of the phosphorus-free alkali-resistant solubilizer is 0.5 to 1.5 times of the dosage of the nonionic surfactant.
9. The use of the phosphorus-free alkali-resistant solubilizing agent according to claim 8, wherein the nonionic surfactant comprises alkylphenol ethoxylates, fatty alcohol ethoxylates, alkylphenol polyoxyethylene/propylene block polyethers, fatty alcohol polyoxyethylene/propylene block polyethers.
10. The use of the phosphorus-free alkali-resistant solubilizing agent according to claim 8, wherein the salt solution has a concentration of 5 to 25%, and the salt in the salt solution comprises (meta) sodium silicate, sodium citrate, borate, chromate, manganate; the concentration of the alkali solution is 5-25%, and the alkali in the alkali solution comprises KOH, NaOH and Na2CO3
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Denomination of invention: A phosphorus free alkali resistant solvent and its preparation and application

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