CN112194600A - Method for synthesizing sulfuric acid mono-alkyl ester lithium salt with low cost - Google Patents
Method for synthesizing sulfuric acid mono-alkyl ester lithium salt with low cost Download PDFInfo
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- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
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Abstract
The invention relates to the field of lithium salt synthesis, and discloses a method for synthesizing a monoalkyl sulfate lithium salt at low cost. The method for synthesizing the monoalkyl sulfate lithium salt at low cost comprises the following steps: (1) mixing alcohols and sulfonyl compounds, stirring at 10-200 deg.C and 0-2Mpa for 2-48 hr; (2) adding a lithium salt compound into the mixed solution obtained in the step (1), and reacting for 2-48 hours at 20-200 ℃ and 0-2 MPa; (3) after the reaction of step (2), the monoalkyl sulfate lithium salt is obtained by purification. The method utilizes the reaction of lithium salt compounds, sulfonyl substances and alcohols in a solvent to obtain the monoalkyl sulfate lithium salt, has simple and easily obtained raw materials, is easy to store, and is suitable for the synthesis of various monoalkyl sulfate lithium salts.
Description
Technical Field
The invention relates to the field of lithium salt synthesis, in particular to a method for synthesizing a monoalkyl sulfate lithium salt at low cost.
Background
The sulfuric acid monoalkyl ester salt can be used as a detergent, a wetting agent, a foaming agent, an emulsifier and the like, is commonly used in industrial cleaning agents and household detergents, and is also used in industries of cosmetics, textiles, metal processing, printing and dyeing and the like. At present, the preparation method of the relatively common sulfuric acid monoalkyl ester salt mainly comprises two methods: one is to directly prepare the sulfuric acid monohydroxyl ester salt by neutralizing the sulfuric acid monohydroxyl ester with alkali; the other method is to carry out alkylation reaction on dialkyl sulfate and organic amine to obtain ammonium salt of the dialkyl sulfate, and then react the ammonium salt with corresponding salt. In both methods, the hydrocarbyl sulfate is required to be directly used, raw materials are not easy to obtain, and the hydrocarbyl sulfate is harsh in storage conditions and easy to deteriorate.
The sulfuric acid mono-alkyl ester lithium salt compound is used as a lithium ion battery non-aqueous electrolyte additive, is used in a lithium ion battery, can form a low-molecular organic lithium salt component with low impedance and good lithium ion permeability on the surface of a pole piece, effectively protects the contact decomposition between an electrolyte and the pole piece, reduces the impedance of the battery, improves the low-temperature performance and the cycle performance of the battery, has large usage amount in the field of the lithium ion battery, and develops a method for synthesizing the sulfuric acid mono-alkyl ester lithium salt with low cost, which is beneficial to promoting the development of the lithium ion battery and reducing the cost of the lithium ion battery.
Disclosure of Invention
The invention provides a method for synthesizing a mono-alkyl sulfate lithium salt at low cost, aiming at overcoming the defects of synthesizing the mono-alkyl sulfate lithium salt in the prior art and reducing the cost of a lithium ion battery.
To achieve the object of the present invention, the low-cost method for synthesizing a lithium salt of a monoalkyl sulfate according to the present invention comprises the steps of:
(1) mixing alcohol substances, sulfonyl substances and solvents;
(2) adding a lithium salt compound into the mixed solution obtained in the step (1);
(3) after the reaction of step (2), the monoalkyl sulfate lithium salt is obtained by purification.
Preferably, in the step (1), the alcohol substance and the sulfonyl substance are stirred for 2 to 48 hours at a temperature of between 10 and 200 ℃ and under a pressure of between 0 and 2 MPa.
Further, in the step (1), the molar ratio of the alcohol substance to the sulfonyl substance is 40: 1-2: 1.
Further, the alcohol substance in the step (1) is selected from at least one of the following formulas 1:
R1-OH
formula 1
Wherein R is1Is an alkyl, alkenyl or alkynyl group having 20 or less carbon atoms, for example, an alkyl, alkenyl or alkynyl group having 1 to 5 carbon atoms.
Further, the sulfonyl-type substance in the step (1) is selected from at least one of formula 2:
wherein, X1、X2Is a halogen atom or a hydroxyl group, and X1、X2Not simultaneously being hydroxyl.
Preferably, the lithium salt compound is added in the step (2) and then the reaction is carried out for 2 to 48 hours at the temperature of 20 to 200 ℃ and under the pressure of 0 to 2 MPa.
Further, the lithium salt compound in the step (2) is one or more selected from lithium hydroxide, lithium fluoride, lithium chloride, lithium carbonate, lithium acetate and lithium oxalate.
Further, the molar ratio of the lithium content of the lithium salt compound in the step (2) to the sulfonyl compound in the step (1) is 1:1-1: 10.
Further, in the step (3), the purification is to separate the unnecessary alcohol substance and the solvent by distillation under reduced pressure to obtain a mixture of the monoalkyl sulfate lithium salt and high-boiling impurities, to remove the high-boiling impurities by washing with a nonpolar solvent, and to dry at 20 to 100 ℃ under a pressure of 60Kpa to further purify the product to obtain the monoalkyl sulfate lithium salt.
In the present invention, preferably, the alcohol is methanol, ethanol, methallyl alcohol or isopropanol; the sulfonyl substances are sulfonyl chloride or chlorosulfonic acid; the lithium salt compound is lithium acetate, lithium carbonate or lithium oxalate, and more preferably, the alcohol substance, the sulfonyl substance and the lithium salt compound are methallyl alcohol, sulfonyl chloride and lithium carbonate, or ethanol, chlorosulfonic acid and lithium carbonate.
The method of the invention utilizes the reaction of lithium salt compounds, sulfonyl substances and alcohols in the solvent to obtain the sulfuric acid monoalkyl ester lithium salt, the raw materials are simple and easy to obtain and store, and the method is suitable for the synthesis of various types of sulfuric acid monoalkyl ester lithium salts, and provides a brand new way for preparing high-quality sulfuric acid monoalkyl ester salts.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
Further, the technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
The method of the invention utilizes the reaction of lithium salt compounds, sulfonyl substances and alcohols in the solvent to obtain the sulfuric acid monoalkyl ester lithium salt, the raw materials are simple and easy to obtain and easy to store, and a brand new way is provided for preparing the high-quality sulfuric acid monoalkyl ester salt. Wherein the solvent is only a raw material for dispersing reaction so as to facilitate the reaction of the two, therefore, the solvent which can achieve the effect can be used; of course, it is preferable not to use an aqueous solvent in order not to introduce water. In addition, in view of the ease of solvent removal, several alcohols are preferred as starting materials in the examples of the present invention, and these alcohols can be used as both starting materials and solvents in the present invention.
Example one
Weighing 15mol of absolute ethyl alcohol, mixing the absolute ethyl alcohol with 1mol of sulfonyl chloride, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.8mol of lithium acetate, adding the lithium acetate into the mixed solution, and stirring and reacting for 4 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive ethanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken out and dried at 40 ℃ under a pressure of 40kPa for 8 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 78.9%, the water content was 25.6ppm, the acidity was 189ppm, and Cl was found-Less than 1ppm, and anion chromatography detection content of 99.5%.
Example two
Weighing 14mol of absolute ethyl alcohol, mixing the absolute ethyl alcohol with 1mol of sulfonyl chloride, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium carbonate, adding the lithium carbonate into the mixed solution, and stirring and reacting for 6 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive ethanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. After detection, this exampleThe yield of the monohydrocarbyl sulfate lithium salt (b) was 89.6%, the water content was 13.7ppm, the acidity was 131ppm, and Cl was-Less than 1ppm, and anion chromatography detection content of 99.3%.
EXAMPLE III
Weighing 15mol of anhydrous methanol, mixing the anhydrous methanol with 1mol of sulfonyl chloride, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium carbonate, adding the lithium carbonate into the mixed solution, and stirring and reacting for 6 hours at 90 ℃ under the protection of nitrogen and reflux; evaporating excessive methanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 90.7%, the water content was 30.4ppm, the acidity was 120ppm, and Cl was found to be-Less than 1ppm, and anion chromatography detection content of 99.7%.
Example four
Weighing 15mol of anhydrous methanol, mixing the anhydrous methanol with 1mol of sulfonyl chloride, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.8mol of lithium acetate, adding the lithium acetate into the mixed solution, and stirring and reacting for 4 hours at 80 ℃ under the protection of nitrogen and reflux; evaporating excessive methanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of detection, the yield of the monohydrocarbyl sulfate lithium salt in this example was 80.1%, the water content was 20.1ppm, the acidity was 173ppm, and Cl was found to be-Less than 1ppm, and anion chromatography detection content of 99.5%.
EXAMPLE five
Weighing 15mol of anhydrous methallyl alcohol, mixing the anhydrous methallyl alcohol with 1mol of sulfonyl chloride, and stirring for 4 hours at the temperature of 60 ℃ under the protection of nitrogen; weighing 0.4mol of lithium carbonate, adding the lithium carbonate into the mixed solution, and stirring and reacting for 6 hours at the temperature of 120 ℃ under the protection of nitrogen and under reflux; evaporating excessive methallyl alcohol by a reduced pressure distillation mode to obtain a crude product; washing the crude product with dichloromethane in a glove box for 3 times, filtering, collecting solid, drying at 70 deg.C under 20kPa for 4 hr to obtain high purityA lithium salt of a monohydrocarbyl sulfate of (1). As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt was 92.3% in this example, the water content was 28.4ppm, the acidity was 111ppm, and Cl was measured-Less than 1ppm, and anion chromatography detection content of 99.8%.
EXAMPLE six
Weighing 15mol of anhydrous methallyl alcohol, mixing the anhydrous methallyl alcohol with 1mol of sulfonyl chloride, and stirring for 4 hours at the temperature of 60 ℃ under the protection of nitrogen; weighing 0.8mol of lithium acetate, adding the lithium acetate into the mixed solution, and stirring and reacting for 6 hours at the temperature of 120 ℃ under the protection of nitrogen and under reflux; evaporating excessive methallyl alcohol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken out and dried at 70 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of detection, the yield of the monohydrocarbyl sulfate lithium salt in this example was 81.4%, the water content was 23.7ppm, the acidity was 142ppm, and Cl was found-Less than 1ppm, and anion chromatography detection content of 99.7%.
EXAMPLE seven
Weighing 15mol of anhydrous isopropanol, mixing the anhydrous isopropanol with 1mol of sulfonyl chloride, and stirring for 4 hours at the temperature of 60 ℃ under the protection of nitrogen; weighing 0.4mol of lithium carbonate, adding the lithium carbonate into the mixed solution, and stirring and reacting for 4 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive isopropanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 89.4%, the water content was 22.2ppm, the acidity was 157ppm, and Cl was found to be-Less than 1ppm, and anion chromatography detection content of 99.8%.
Example eight
Weighing 15mol of anhydrous isopropanol, mixing the anhydrous isopropanol with 1mol of sulfonyl chloride, and stirring for 4 hours at the temperature of 60 ℃ under the protection of nitrogen; weighing 0.8mol of lithium acetate, adding the lithium acetate into the mixed solution, and stirring and reacting for 4 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive isopropanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed 3 times with dichloromethane in a glove box and filteredAnd drying the solid at 50 ℃ under the pressure of 20kPa for 4 hours to obtain the high-purity lithium salt of the monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt was 77.7% in this example, the water content was 34.1ppm, the acidity was 180ppm, and Cl was measured-Less than 1ppm, and anion chromatography detection content of 99.5%.
Example nine
Weighing 15mol of absolute ethyl alcohol, mixing the absolute ethyl alcohol with 1mol of chlorosulfonic acid, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium carbonate, adding the lithium carbonate into the mixed solution, and stirring and reacting for 4 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive ethanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. The yield of the monohydrocarbyl sulfate lithium salt in this example was found to be 97.6%, the water content was 21.1ppm, the acidity was 109ppm, and Cl was found to be-Less than 1ppm, and anion chromatography detection content of 99.5%.
Example ten
Weighing 15mol of absolute ethyl alcohol, mixing the absolute ethyl alcohol with 1mol of chlorosulfonic acid, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.8mol of lithium acetate, adding the lithium acetate into the mixed solution, and stirring and reacting for 4 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive ethanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 87.5%, the water content was 19.8ppm, the acidity was 97ppm, and Cl was found to be-Less than 1ppm, and anion chromatography detection content of 99.6%.
EXAMPLE eleven
Weighing 15mol of anhydrous methanol, mixing the anhydrous methanol with 1mol of chlorosulfonic acid, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium carbonate, adding the lithium carbonate into the mixed solution, and stirring and reacting for 4 hours at 80 ℃ under the protection of nitrogen and reflux; evaporating excessive methanol by a reduced pressure distillation mode to obtain a crude product; in a glove box, using dichloro chlorideThe crude product was washed with methane 3 times, filtered, and the solid was taken and dried at 50 ℃ under 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 88.4%, the water content was 20.1ppm, the acidity was 119ppm, and Cl was found-Less than 1ppm, and anion chromatography detection content of 99.7%.
Example twelve
Weighing 15mol of anhydrous methanol, mixing the anhydrous methanol with 1mol of chlorosulfonic acid, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.8mol of lithium acetate, adding the lithium acetate into the mixed solution, and stirring and reacting for 4 hours at 80 ℃ under the protection of nitrogen and reflux; evaporating excessive methanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of detection, the yield of the monohydrocarbyl sulfate lithium salt in this example was 81.4%, the water content was 16.7ppm, the acidity was 153ppm, and Cl was found to be-Less than 1ppm, and anion chromatography detection content of 99.7%.
EXAMPLE thirteen
Weighing 15mol of absolute ethyl alcohol, mixing the absolute ethyl alcohol with 1mol of sulfonyl chloride, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium oxalate, adding the lithium oxalate into the mixed solution, and stirring and reacting for 4 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive ethanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 87.4%, the water content was 24.1ppm, the acidity was 132ppm, and Cl was measured-Less than 1ppm, and anion chromatography detection content of 99.5%.
Example fourteen
Weighing 15mol of anhydrous methanol, mixing the anhydrous methanol with 1mol of sulfonyl chloride, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium oxalate, adding the lithium oxalate into the mixed solution, and stirring and reacting for 4 hours at 80 ℃ under the protection of nitrogen and reflux; distilling off excessive methanol by reduced pressure distillation to obtainA crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 89.6%, the water content was 39.7ppm, the acidity was 155ppm, and Cl was found-Less than 1ppm, and anion chromatography detection content of 99.8%.
Example fifteen
Weighing 15mol of absolute ethyl alcohol, mixing the absolute ethyl alcohol with 1mol of chlorosulfonic acid, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium oxalate, adding the lithium oxalate into the mixed solution, and stirring and reacting for 4 hours at 100 ℃ under the protection of nitrogen and reflux; evaporating excessive ethanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 88.1%, the water content was 27.6ppm, the acidity was 87ppm, and Cl was measured-Less than 1ppm, and anion chromatography detection content of 99.5%.
Example sixteen
Weighing 15mol of anhydrous methanol, mixing the anhydrous methanol with 1mol of chlorosulfonic acid, and stirring for 4 hours at 40 ℃ under the protection of nitrogen; weighing 0.4mol of lithium oxalate, adding the lithium oxalate into the mixed solution, and stirring and reacting for 4 hours at 80 ℃ under the protection of nitrogen and reflux; evaporating excessive methanol by a reduced pressure distillation mode to obtain a crude product; the crude product was washed with dichloromethane 3 times in a glove box, filtered, and the solid was taken and dried at 50 ℃ under a pressure of 20kPa for 4 hours to obtain a high-purity lithium salt of monoalkyl sulfate. As a result of examination, the yield of the monohydrocarbyl sulfate lithium salt in this example was 89.2%, the water content was 31.0ppm, the acidity was 111ppm, and Cl was measured-Less than 1ppm, and anion chromatography detection content of 99.5%.
The specific reaction conditions and parameters for the above examples are shown in the following table:
it will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.
Claims (10)
1. A method for synthesizing a monohydrocarbyl sulfate lithium salt at low cost, the method comprising the steps of:
(1) mixing alcohol substances, sulfonyl substances and solvents;
(2) adding a lithium salt compound into the mixed solution obtained in the step (1);
(3) after the reaction of step (2), the monoalkyl sulfate lithium salt is obtained by purification.
2. The method for synthesizing the lithium salt of monoalkyl sulfate at low cost according to claim 1, wherein the alcohol and the sulfonyl are stirred at 10 to 200 ℃ and 0 to 2Mpa for 2 to 48 hours in the step (1).
3. The method for synthesizing the lithium salt of mono-alkyl sulfate at low cost according to claim 1, wherein the molar ratio of the alcohol to the sulfonyl compound in step (1) is 40:1 to 2: 1.
4. The method for synthesizing the lithium salt of mono-hydrocarbyl sulfate at low cost according to claim 1, characterized in that the alcohol in step (1) is selected from at least one of the following formulas 1:
R1-OH
formula 1
Wherein R is1Is an alkyl, alkenyl or alkynyl group having 20 or less carbon atoms, for example, an alkyl, alkenyl or alkynyl group having 1 to 5 carbon atoms.
5. The method for synthesizing the lithium salt of monoalkyl sulfate according to claim 1, wherein the sulfonyl species in step (1) is selected from at least one of formula 2:
wherein, X1、X2Is a halogen atom or a hydroxyl group, and X1、X2Not simultaneously being hydroxyl.
6. The method for synthesizing the lithium salt of monoalkyl sulfate at low cost according to claim 1, wherein the step (2) comprises the step of adding a lithium salt-like compound and then reacting at 20 to 200 ℃ and 0 to 2MPa for 2 to 48 hours.
7. The method for synthesizing the lithium salt of mono-alkyl sulfate at low cost according to claim 1, wherein the lithium salt compound in the step (2) is one or more selected from the group consisting of lithium hydroxide, lithium fluoride, lithium chloride, lithium carbonate, lithium acetate and lithium oxalate.
8. The method for synthesizing the lithium salt of mono-hydrocarbyl sulfate at low cost according to claim 1, characterized in that the molar ratio of the lithium content of the lithium salt-based compound in the step (2) to the sulfonyl-based compound in the step (1) is 1:1 to 1: 10.
9. The method for synthesizing the monoalkyl sulfate lithium salt at low cost according to claim 1, wherein in the step (3), the purification is carried out by separating the excess alcohol and the solvent by distillation under reduced pressure to obtain a mixture of the monoalkyl sulfate lithium salt and the high-boiling impurities, washing with a nonpolar solvent to remove the high-boiling impurities, and drying at 20 to 100 ℃ under a pressure of 60Kpa to further purify the product to obtain the monoalkyl sulfate lithium salt.
10. The method for low-cost synthesis of lithium monoalkyl sulfate according to claim 1, wherein the alcohol is methanol, ethanol, methallyl alcohol or isopropanol, the sulfonyl is sulfonyl chloride or chlorosulfonic acid, and the lithium salt is lithium acetate, lithium carbonate or lithium oxalate, preferably the alcohol, sulfonyl and lithium salt are methallyl alcohol, sulfonyl chloride, lithium carbonate, or ethanol, chlorosulfonic acid or lithium carbonate.
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Application publication date: 20210108 |