CN113680274B - Preparation method of compound alcohol ether carboxylate - Google Patents
Preparation method of compound alcohol ether carboxylate Download PDFInfo
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- CN113680274B CN113680274B CN202110979395.4A CN202110979395A CN113680274B CN 113680274 B CN113680274 B CN 113680274B CN 202110979395 A CN202110979395 A CN 202110979395A CN 113680274 B CN113680274 B CN 113680274B
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Abstract
The invention discloses a preparation method of a composite alcohol ether carboxylate, which belongs to the technical field of surfactant preparation and is used for obtaining an alcohol ether carboxylate surfactant with better quality.A component A and a component B are synthesized, and then an aqueous solution of the component A and an aqueous solution of the component B are mixed in proportion to prepare the composite alcohol ether carboxylate; the component A is an alcohol ether carboxylate, the component B is a quaternary ammonium salt compound, the component A uses isomeric tridecanol polyoxyethylene ether as a raw material, so that the surfactant has good alkali resistance and oxidation resistance, and is milder, the component B is prepared by a series of synthesis, is a biquaternary ammonium salt compound with long carbon chains at two ends, has various performances such as antistatic and antibacterial properties, and the like, and after the component A and the component B are compounded, the obtained compound alcohol ether carboxylate has better antibacterial performance, salt resistance and the like and has higher surface activity.
Description
Technical Field
The invention relates to the technical field of surfactant preparation, in particular to a preparation method of a compound alcohol ether carboxylate.
Background
The Alcohol Ether Carboxylate (AEC) is a novel anionic surfactant, has the characteristics of other anionic surfactants, such as low toxicity, easy biodegradation, low surface tension, good compatibility with other surfactants and the like, and is a multifunctional green surfactant. Due to its special properties, fatty alcohol ether carboxylates have found wide application in the fields of cosmetics, detergents, biochemistry, plastics, leather, pharmaceuticals, food processing and the petroleum industry.
The alcohol ether carboxylate is prepared by embedding certain addition number of polyoxyethylene (EO) between hydrophilic group and hydrophobic group of soap, and the introduction of EO chain makes alcohol ether carboxylate have better water solubility, calcium soap dispersibility and hard water resistance than soap. The alcohol ether carboxylate has the characteristics of both anionic surfactant and nonionic surfactant, can prepare products with different characteristics by adjusting the length of a hydrophobic group chain, the addition number of EO and pH, has good compatibility, and can be compounded with other various surfactants to ensure that the products have better quality.
Disclosure of Invention
Technical problem to be solved
The invention provides a preparation method of a composite alcohol ether carboxylate, which is used for obtaining an alcohol ether carboxylate surfactant with better quality.
(II) technical scheme
In order to realize the purpose, the invention is realized by the following technical scheme: the preparation method of the complex alcohol ether carboxylate comprises the following steps:
the method comprises the following steps: adding the component A into a stirring kettle filled with deionized water, and stirring for 20min at 50-60 ℃ and 500-700r/min to obtain solution A;
step two: adding the component B into another stirring kettle filled with deionized water, and stirring for 15min at 60-70 deg.C and rotation speed of 800-1000r/min to obtain solution B;
step three: adding the solution A obtained in the step one and the solution B obtained in the step two into a reaction kettle, and stirring and mixing for 15-25min at the temperature of 20-30 ℃ and the rotating speed of 400-600r/min to obtain compound alcohol ether carboxylate;
wherein the component B is prepared by the following steps:
step B1: adding p-xylene, deionized water and potassium permanganate into a clean and dry flask, heating to 110-120 ℃, carrying out reflux reaction for 3-4h to obtain an intermediate 1, then adding the intermediate 1 and deionized water into the clean and dry flask, stirring for 10-20min at the temperature of 50 ℃ and the rotation speed of 200r/min, then adding thionyl chloride and a catalyst, heating to 70 ℃, carrying out reflux reaction for 5-7h, reducing pressure after the reaction is finished to remove unreacted thionyl chloride, and carrying out rotary evaporation to obtain an intermediate 2;
the reaction equation is as follows:
and step B2: adding dichloromethane into a clean and dry flask, then adding 4- (bromomethyl) aniline and triethylamine into the flask, adding a dichloromethane solution of an intermediate 2 into the flask by using a dropping funnel under an ice bath condition, stirring and reacting for 2-3h at the temperature of 20-30 ℃ and the rotating speed of 500r/min after the dropwise addition is finished, and washing and drying to obtain an intermediate 3 after the reaction is finished;
and step B3: adding dimethylformamide into a clean and dry flask, then adding chlorododecane, stirring for 10min at the temperature of 100-110 ℃ and the rotation speed of 500r/min, dropping dimethylamine into the flask by using a dropping funnel under the condition after stirring, reacting for 2-3h at the temperature of 105 ℃ and the rotation speed of 500-700r/min after dropping, and performing rotary evaporation to remove a solvent after the reaction is finished to obtain an intermediate 4;
the reaction equation is as follows:
and step B4: and (3) adding dimethyl sulfoxide into a clean and dry flask, then adding the intermediate 3 obtained in the step B2 and the intermediate 4 obtained in the step B3 into the flask, stirring and reacting for 2-3h at the temperature of 80 ℃ and the rotating speed of 600-800r/min, removing the solvent by rotary evaporation after the reaction is finished, and drying to obtain the component B.
The reaction equation is as follows:
further, the dosage ratio of the component A to the deionized water in the first step is 20-30g:3.5L; the dosage ratio of the component B to the deionized water in the step two is 15-20g:2.8L; in the third step, the volume ratio of the dosage of the solution A to the dosage of the solution B is 3:1-3.
Further, the dosage ratio of the p-xylene to the potassium permanganate in the step B1 is 1g:2.3g, the dosage ratio of the intermediate 2, the thionyl chloride and the catalyst is 1.7g:3.5g:0.5g, the catalyst is N, N-dimethylformamide.
Further, the amount ratio of the dichloromethane solution of dichloromethane, 4- (bromomethyl) aniline, triethylamine and intermediate 2 in the step B2 is 50mL:1.6g:0.3g:39mL, wherein the dichloromethane solution of the intermediate 2 is the mixture of the intermediate 2 and dichloromethane in a dosage ratio of 1.1g:15mL of the above-mentioned components were mixed together to prepare a mixture.
Further, in the step B3, the dosage ratio of dimethylformamide, chlorododecane and dimethylamine is 50mL:3g:0.8g.
Further, the dosage ratio of the dimethyl sulfoxide, the intermediate 3 and the intermediate 4 in the step B4 is 45mL:2.3g:1.6g.
Further, component a is made by the steps of:
step A1: adding isomeric tridecanol polyoxyethylene ether into a reaction kettle which is cleaned and dried, stirring for 20-30min at the temperature of 40-50 ℃ and the rotating speed of 800-900r/min, then adding chloroacetic acid into the reaction kettle while keeping the conditions unchanged, keeping the rotating speed unchanged after the addition is finished, heating to 60 ℃, adding sodium hydroxide powder, and reacting for 30-50min;
step A2: continuously adding chloroacetic acid and sodium hydroxide powder into the system, continuously reacting for 5-6h at the temperature of 60 ℃ and the rotating speed of 500-700r/min, adding anhydrous ethanol at the temperature of 60 ℃ after the reaction is finished, then carrying out suction filtration, recrystallizing the obtained solid for 3 times by using the anhydrous ethanol after the filtrate is subjected to rotary evaporation, and drying to obtain the component A.
Further, the EO number of the isomeric tridecanol polyoxyethylene ether in the step A1 is 5, and the dosage ratio of the isomeric tridecanol polyoxyethylene ether, the chloroacetic acid and the sodium hydroxide powder in the step A1 is 1mL:1g:0.6g, wherein the dosage ratio of chloroacetic acid to sodium hydroxide in the step A2 is 1g:0.6g, chloroacetic acid and sodium hydroxide were used in the same amount as in step A1 in step A2.
(III) advantageous effects
The invention provides a preparation method of a compound alcohol ether carboxylate. Compared with the prior art, the method has the following beneficial effects: synthesizing a component A and a component B, and mixing aqueous solutions of the component A and the component B in proportion to prepare a composite alcohol ether carboxylate; wherein the component A is alcohol ether carboxylate, and the component B is a quaternary ammonium salt compound;
the component A is synthesized by taking isomeric tridecanol polyoxyethylene ether with EO number of 5 as a raw material to react with sodium hydroxide step by step under the action of chloroacetic acid to synthesize isomeric alcohol ether carboxylate with EO number of 5, wherein EO-based ethylene oxide is hydrophilic group and is introduced into the molecule of the alcohol ether carboxylate, so that the surfactant has good alkali resistance and oxidation resistance, is milder, has the characteristics of anionic surfactant and nonionic surfactant, and has good compatibility;
the synthesis of the component B takes p-xylene as a raw material, two hydroxyl groups of the p-xylene are oxidized into carboxyl groups in a potassium permanganate solution to form terephthalic acid, the p-dibenzoic acid reacts with thionyl chloride under a catalyst to generate substitution reaction to generate terephthaloyl chloride, then the p-dibenzoyl chloride reacts with 4- (bromomethyl) aniline, the acid chloride group of the p-dibenzoyl chloride reacts with the amino group of the 4- (bromomethyl) aniline to generate an intermediate 3 with bromobenzyl at two ends, then chlorododecane and dimethylamine are subjected to alkylation reaction to generate the intermediate 4, the intermediate 4 and the intermediate 3 are subjected to quaternization reaction in a solvent to generate a biquaternary ammonium salt compound with tetradecyl at two ends, the quaternary ammonium compound has good antibacterial and antistatic effects and can adsorb substances with negative surface charges, the long carbon chains at two ends are hydrophobic ends, and the dodecane also has good antibacterial effects, a cationic hydrophilic group is connected with two hydrophobic chains, and a connecting group in the middle reduces repulsive force between two polar head groups and acting force between the hydrophobic chains, so that the component B can be closely arranged in an aqueous solution, and molecules are more easily aggregated in a surface layer system to form a solution with high surface adsorption capacity and high aggregation capability.
The component A and the component B are compounded to obtain the compound alcohol ether carboxylate which has the characteristics of the component A and the component B at the same time, so that the softer compound surfactant is obtained, is mild and non-irritant, has excellent antibacterial performance and antistatic capability, and obtains a surfactant with better quality.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation of the component A comprises the following steps:
step A1: adding isomeric tridecanol polyoxyethylene ether into a reaction kettle which is cleaned and dried, stirring for 20min at the temperature of 40 ℃ and the rotating speed of 800r/min, then keeping the conditions unchanged, adding chloroacetic acid into the reaction kettle, keeping the rotating speed unchanged after the addition is finished, heating to 60 ℃, adding sodium hydroxide powder, and reacting for 30min;
step A2: and continuously adding chloroacetic acid and sodium hydroxide powder into the system, continuously reacting for 5h at the temperature of 60 ℃ and the rotating speed of 500r/min, adding absolute ethyl alcohol at the temperature of 60 ℃ after the reaction is finished, then carrying out suction filtration, recrystallizing the solid obtained after the filtrate is subjected to rotary evaporation for 3 times by using the absolute ethyl alcohol, and drying to obtain the component A.
Example 2
The preparation of the component A comprises the following steps:
step A1: adding isomeric tridecanol polyoxyethylene ether into a reaction kettle which is cleaned and dried, stirring for 25min at the temperature of 45 ℃ and the rotating speed of 850r/min, then adding chloroacetic acid into the reaction kettle under the condition of keeping the condition unchanged, keeping the rotating speed unchanged after the addition is finished, heating to 60 ℃, adding sodium hydroxide powder, and reacting for 40min;
step A2: and continuously adding chloroacetic acid and sodium hydroxide powder into the system, continuously reacting for 5.5 hours at the temperature of 60 ℃ and the rotating speed of 600r/min, adding absolute ethyl alcohol at the temperature of 60 ℃ after the reaction is finished, then performing suction filtration, performing rotary evaporation on the filtrate to obtain a solid, recrystallizing for 3 times by using the absolute ethyl alcohol, and drying to obtain the component A.
Example 3
The preparation of the component A comprises the following steps:
step A1: adding isomeric tridecanol polyoxyethylene ether into a reaction kettle which is cleaned and dried, stirring for 30min at the temperature of 50 ℃ and the rotating speed of 900r/min, then adding chloroacetic acid into the reaction kettle under the condition of keeping the condition unchanged, keeping the rotating speed unchanged after the addition is finished, heating to 60 ℃, adding sodium hydroxide powder, and reacting for 50min;
step A2: and continuously adding chloroacetic acid and sodium hydroxide powder into the system, continuously reacting for 6 hours at the temperature of 60 ℃ and the rotating speed of 700r/min, adding absolute ethyl alcohol at the temperature of 60 ℃ after the reaction is finished, then performing suction filtration, performing rotary evaporation on the filtrate to obtain a solid, recrystallizing for 3 times by using the absolute ethyl alcohol, and drying to obtain the component A.
Example 4
The preparation of the component B specifically comprises the following steps:
step B1: adding p-xylene, deionized water and potassium permanganate into a clean and dry flask, heating to 110 ℃, carrying out reflux reaction for 3 hours to obtain an intermediate 1, then adding the intermediate 1 and deionized water into the clean and dry flask, stirring for 10 minutes at the temperature of 50 ℃ and the rotation speed of 200r/min, then adding thionyl chloride and a catalyst into the flask, heating to 70 ℃, carrying out reflux reaction for 5 hours, reducing pressure after the reaction is finished to remove unreacted thionyl chloride, and carrying out rotary evaporation to obtain an intermediate 2;
and step B2: adding dichloromethane into a clean and dry flask, then adding 4- (bromomethyl) aniline and triethylamine into the flask, adding a dichloromethane solution of an intermediate 2 into the flask by using a dropping funnel under an ice bath condition, stirring and reacting for 2 hours at the temperature of 20 ℃ and the rotating speed of 500r/min after the dropwise addition is finished, and washing and drying to obtain an intermediate 3 after the reaction is finished;
and step B3: adding dimethylformamide into a clean and dry flask, then adding chlorododecane, stirring for 10min at the temperature of 100 ℃ and the rotation speed of 500r/min, dropping dimethylamine into the flask by using a dropping funnel under the condition after stirring, reacting for 2h at the temperature of 105 ℃ and the rotation speed of 500r/min after dropping, and performing rotary evaporation to remove a solvent after the reaction is finished to obtain an intermediate 4;
and step B4: adding dimethyl sulfoxide into a clean and dry flask, then adding the intermediate 3 obtained in the step B2 and the intermediate 4 obtained in the step B3 into the flask, stirring and reacting for 2 hours at the temperature of 80 ℃ and the rotation speed of 600r/min, removing the solvent by rotary evaporation after the reaction is finished, and drying to obtain the component B.
Example 5
The preparation of the component B specifically comprises the following steps:
step B1: adding p-xylene, deionized water and potassium permanganate into a clean and dry flask, heating to 115 ℃, carrying out reflux reaction for 3.5 hours to obtain an intermediate 1, then adding the intermediate 1 and deionized water into the clean and dry flask, stirring for 15 minutes at the temperature of 50 ℃ and the rotating speed of 200r/min, then adding thionyl chloride and a catalyst, heating to 70 ℃, carrying out reflux reaction for 6 hours, carrying out reduced pressure removal on the incompletely reacted thionyl chloride after the reaction is finished, and carrying out rotary evaporation to obtain an intermediate 2;
and step B2: adding dichloromethane into a clean and dry flask, then adding 4- (bromomethyl) aniline and triethylamine into the flask, adding a dichloromethane solution of an intermediate 2 into the flask by using a dropping funnel under an ice bath condition, stirring and reacting for 2.5 hours at the temperature of 25 ℃ and the rotating speed of 500r/min after the dropwise addition is finished, and washing and drying to obtain an intermediate 3 after the reaction is finished;
and step B3: adding dimethylformamide into a clean and dry flask, then adding chlorododecane, stirring for 10min at the temperature of 105 ℃ and the rotation speed of 500r/min, dropping dimethylamine into the flask by using a dropping funnel under the condition after stirring, reacting for 2.5h at the temperature of 105 ℃ and the rotation speed of 600r/min after dropping, and performing rotary evaporation to remove a solvent after the reaction is finished to obtain an intermediate 4;
and step B4: adding dimethyl sulfoxide into a clean and dry flask, then adding the intermediate 3 obtained in the step B2 and the intermediate 4 obtained in the step B3 into the flask, stirring and reacting for 2.5h at the temperature of 80 ℃ and the rotation speed of 700r/min, removing the solvent by rotary evaporation after the reaction is finished, and drying to obtain the component B.
Example 6
The preparation of the component B specifically comprises the following steps:
step B1: adding p-xylene, deionized water and potassium permanganate into a clean and dry flask, heating to 120 ℃, carrying out reflux reaction for 4 hours to obtain an intermediate 1, then adding the intermediate 1 and deionized water into the clean and dry flask, stirring for 20 minutes at the temperature of 50 ℃ and the rotating speed of 200r/min, then adding thionyl chloride and a catalyst into the flask, heating to 70 ℃, carrying out reflux reaction for 7 hours, reducing pressure after the reaction is finished to remove unreacted thionyl chloride, and carrying out rotary evaporation to obtain an intermediate 2;
and step B2: adding dichloromethane into a clean and dry flask, then adding 4- (bromomethyl) aniline and triethylamine into the flask, adding a dichloromethane solution of an intermediate 2 into the flask by using a dropping funnel under an ice bath condition, stirring and reacting for 3 hours at the temperature of 30 ℃ and the rotating speed of 500r/min after the dropwise addition is finished, and washing and drying to obtain an intermediate 3 after the reaction is finished;
and step B3: adding dimethylformamide into a clean and dry flask, then adding chlorododecane, stirring for 10min at the temperature of 110 ℃ and the rotation speed of 500r/min, dropping dimethylamine into the flask by using a dropping funnel under the condition after stirring, reacting for 3h at the temperature of 105 ℃ and the rotation speed of 700r/min after dropping, and performing rotary evaporation to remove a solvent after the reaction is finished to obtain an intermediate 4;
and step B4: adding dimethyl sulfoxide into a clean and dry flask, then adding the intermediate 3 obtained in the step B2 and the intermediate 4 obtained in the step B3 into the flask, stirring and reacting for 3 hours at the temperature of 80 ℃ and the rotation speed of 800r/min, removing the solvent by rotary evaporation after the reaction is finished, and drying to obtain the component B.
Example 7
A complex alcohol ether carboxylate is prepared by the following steps:
the method comprises the following steps: adding the component A into a stirring kettle filled with deionized water, and stirring for 20min at the temperature of 50 ℃ and the rotating speed of 500r/min to obtain a solution A;
step two: adding the component B into another stirring kettle filled with deionized water, and stirring for 15min at the temperature of 60 ℃ and the rotating speed of 800r/min to obtain a solution B;
step three: and adding the solution A obtained in the step one and the solution B obtained in the step two into a reaction kettle, and stirring and mixing for 15min at the temperature of 20 ℃ and the rotating speed of 400r/min to obtain the compound alcohol ether carboxylate.
Example 8
A complex alcohol ether carboxylate is prepared by the following steps:
the method comprises the following steps: adding the component A into a stirring kettle filled with deionized water, and stirring for 20min at the temperature of 55 ℃ and the rotating speed of 600r/min to obtain a solution A;
step two: adding the component B into another stirring kettle filled with deionized water, and stirring for 15min at 65 ℃ and 900r/min to obtain a solution B;
step three: and (3) adding the solution A obtained in the step one and the solution B obtained in the step two into a reaction kettle, and stirring and mixing for 20min at the temperature of 25 ℃ and the rotating speed of 500r/min to obtain the compound alcohol ether carboxylate.
Example 9
A complex alcohol ether carboxylate is prepared by the following steps:
the method comprises the following steps: adding the component A into a stirring kettle filled with deionized water, and stirring for 20min at the temperature of 60 ℃ and the rotating speed of 700r/min to obtain a solution A;
step two: adding the component B into another stirring kettle filled with deionized water, and stirring for 15min at 70 ℃ and 1000r/min to obtain a solution B;
step three: and adding the solution A obtained in the step one and the solution B obtained in the step two into a reaction kettle, and stirring and mixing for 25min at the temperature of 30 ℃ and the rotating speed of 600r/min to obtain the compound alcohol ether carboxylate.
Wherein the components A used in examples 7-9 were prepared according to example 2, the component B was prepared according to example 5, and the volume ratio of the solution A to the solution B was 3:2 and mixing.
Comparative example: no addition of component B compared to example 8.
The examples 7-9 and comparative examples were tested for performance: selecting surface tension, salt resistance and antibacterial performance as test indexes, and specifically comprising the following steps:
surface tension test: surfactant solutions of the same concentration were prepared from the products of examples 7-9 and comparative examples and tested at 25 ℃ using a K12 equilibrium surface tensiometer. The surface tension of the deionized water was measured to 72. + -. 0.5mN/m before the test to debug the instrument. Standing for 3min before each solution is tested, repeatedly measuring the same sample for 3 times, and taking the average value; the results obtained are shown in Table 1:
TABLE 1
It can be seen from the above table that examples 7 to 9 have excellent water surface tension lowering properties and good surface activity as compared with the comparative examples.
And (3) testing salt resistance: the products of examples 7-9 and comparative example were prepared into aqueous solutions of the same concentration, and the same amount of solid inorganic salts NaCl, caCl were added 2 、MgSO 4 Testing 10 groups of different inorganic salt concentrations for each product, after the product is placed at a constant temperature of 45 ℃ for 24 hours, measuring the light transmittance (T) of the solution of the middle layer at a wavelength of 600nm by using a visible spectrophotometer to observe the change of the light transmittance (T) on the concentration of the added inorganic salt, and taking the point with the lowest light transmittance as the tolerance of the product on the electrolyte; the results obtained are shown in table 2:
TABLE 2
| Tolerance ofDegree (g/L) | Example 7 | Example 8 | Example 9 | Comparative example |
| NaCl | 156 | 160 | 157 | 100 |
| CaCl 2 | 134 | 141 | 138 | 15 |
| MgSO 4 | 128 | 132 | 129 | 18 |
It can be seen from the above table that examples 7-9 have good salt tolerance properties, especially for CaCl, compared to the comparative examples 2 With MgSO 4 Has obvious advantages.
And (3) testing antibacterial performance: the bacteriostatic circle method is adopted, the culture days are bacteria 2d, fungi 3d, gram-negative bacteria are escherichia coli, gram-positive bacteria are staphylococcus aureus, spore-forming bacteria are bacillus, fungi are aspergillus flavus, and the obtained results are shown in table 3:
TABLE 3
It can be seen from the above table that examples 7 to 9 have superior antibacterial properties as compared to the comparative example.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The preparation method of the complex alcohol ether carboxylate is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: adding the component A into a stirring kettle filled with deionized water, and stirring to obtain a solution A;
step two: adding the component B into another stirring kettle filled with deionized water, and stirring to obtain a solution B;
step three: adding the solution A and the solution B into a reaction kettle, stirring and mixing to obtain compound alcohol ether carboxylate;
wherein the component B is prepared by the following steps:
step B1: adding paraxylene, deionized water and potassium permanganate into a flask, heating for reflux reaction to obtain an intermediate 1, adding the intermediate 1 and deionized water into another flask, stirring, adding thionyl chloride and a catalyst, heating for reflux reaction, and obtaining an intermediate 2 after the reaction is finished;
and step B2: adding dichloromethane into a flask, adding 4- (bromomethyl) aniline and triethylamine into the flask, then adding a dichloromethane solution of an intermediate 2 into the flask for reaction, and obtaining an intermediate 3 after the reaction is finished;
and step B3: adding dimethylformamide into a flask, then adding chlorododecane, stirring, dripping dimethylamine into the flask for reaction, and obtaining an intermediate 4 after the reaction is finished;
and step B4: adding dimethyl sulfoxide into a flask, then adding an intermediate 3 and an intermediate 4 into the flask, and stirring for reaction to obtain a component B after the reaction is finished, wherein the reaction equation of the component B is as follows:
the component A is prepared by the following steps:
step A1: adding isomeric tridecanol polyoxyethylene ether into a reaction kettle, stirring, adding chloroacetic acid into the reaction kettle, heating, and adding sodium hydroxide powder for reaction;
step A2: continuously adding chloroacetic acid and sodium hydroxide powder into the system, continuously reacting, adding absolute ethyl alcohol with the temperature of 60 ℃ after the reaction is finished, then performing suction filtration, performing rotary evaporation on the filtrate to obtain a solid, recrystallizing for 3 times by using the absolute ethyl alcohol, and drying to obtain a component A;
the reaction equations for intermediate 1 and intermediate 2 are as follows:
the reaction equation for intermediate 3 is as follows:
the reaction equation for intermediate 4 is as follows:
2. the method for preparing the complex alcohol ether carboxylate according to claim 1, wherein: in the first step, the dosage ratio of the component A to deionized water is 20-30g:3.5L; the dosage ratio of the component B to the deionized water in the step two is 15-20g:2.8L; in the third step, the volume ratio of the dosage of the solution A to the dosage of the solution B is 3:1-3.
3. The method for preparing a complex alcohol ether carboxylate as claimed in claim 1, wherein: the dosage ratio of the p-xylene to the potassium permanganate in the step B1 is 1g:2.3g, the dosage ratio of the intermediate 2, the thionyl chloride and the catalyst is 1.7g:3.5g:0.5g, the catalyst was N, N-dimethylformamide.
4. The method for preparing a complex alcohol ether carboxylate as claimed in claim 1, wherein: the dosage ratio of the dichloromethane, the 4- (bromomethyl) aniline, the triethylamine and the dichloromethane solution of the intermediate 2 in the step B2 is 50mL:1.6g:0.3g:39mL, wherein the dichloromethane solution of the intermediate 2 is the mixture of the intermediate 2 and dichloromethane in a dosage ratio of 1.1g:15mL of the above-mentioned mixture was mixed to prepare a mixture.
5. The method for preparing a complex alcohol ether carboxylate as claimed in claim 1, wherein: and in the step B3, the dosage ratio of the dimethylformamide to the chlorododecane to the dimethylamine is 50mL:3g:0.8g.
6. The method for preparing a complex alcohol ether carboxylate as claimed in claim 1, wherein: the dosage ratio of the dimethyl sulfoxide, the intermediate 3 and the intermediate 4 in the step B4 is 45mL:2.3g:1.6g.
7. The method for preparing a complex alcohol ether carboxylate as claimed in claim 1, wherein: the EO number of the isomeric tridecanol polyoxyethylene ether in the step A1 is 5, and the dosage ratio of the isomeric tridecanol polyoxyethylene ether, chloroacetic acid and sodium hydroxide powder in the step A1 is 1mL:1g:0.6g, wherein the dosage ratio of chloroacetic acid to sodium hydroxide in the step A2 is 1g:0.6g, chloroacetic acid and sodium hydroxide used in step A2 were used in the same amounts as in step A1.
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