CN108017563B - Preparation method of ultrahigh-base-number synthetic calcium alkyl benzene sulfonate - Google Patents
Preparation method of ultrahigh-base-number synthetic calcium alkyl benzene sulfonate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
- C10M135/08—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium containing a sulfur-to-oxygen bond
- C10M135/10—Sulfonic acids or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/046—Overbasedsulfonic acid salts
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/04—Groups 2 or 12
Abstract
The invention discloses a preparation method of calcium alkyl benzene sulfonate synthesized by ultrahigh base number, which comprises the steps of adding sulfonic acid, diluent oil, solvent and calcium oxide into a reaction bottle and uniformly mixing; continuously adding an alcohol substance, dodecylphenol or calcium alkylphenol sulfide, an amine substance, calcium chloride and an acid substance into a reaction bottle, carrying out neutralization reaction at 45-55 ℃ for 30-90 minutes, and controlling the pH to be 6-10 after the reaction is finished; adding calcium oxide, water and alcohol substances at one time or multiple times, continuously introducing carbon dioxide for carbonation reaction, and controlling the temperature to be 45-65 ℃ until the carbonation reaction is finished; after the reaction is finished, the materials in the reaction bottle are heated to 70-120 ℃, alcohol substances and water in the materials are distilled out under the vacuum condition of 0-minus 0.09MPa, then the materials are centrifuged to remove residues, and the solvent in the materials is further removed by reduced pressure distillation to obtain the finished product. The invention can prepare the ultra-high base number synthetic calcium sulfonate with TBN600 and calcium content of about 22 percent, and the storage stability of the product diluted into the base oil is good.
Description
Technical Field
The invention relates to the technical field of synthetic calcium sulfonate, in particular to a preparation method of synthetic calcium alkyl benzene sulfonate with an ultrahigh base number.
Background
In the preparation process of the synthetic calcium alkyl benzene sulfonate, the prior art generally adopts one or more times of intermittent addition of a large amount of solid calcium oxide in the carbonation synthesis process, and adopts an intermittent or continuous mode to carry out carbonation reaction, and the base value of the prepared product has low base value (TBN30) calcium alkyl benzene sulfonate, and the calcium content is about 2.0 percent; medium base number (TBN150) calcium alkyl benzene sulfonate, the calcium content is about 6.5 percent; high base number (TBN300) calcium alkyl benzene sulfonate, calcium content is about 12%; the calcium content of the calcium alkyl benzene sulfonate with the ultra-high base number (TBN400) is about 15 percent, and the calcium alkyl benzene sulfonate with the TBN500 can be obtained by a small amount of foreign technologies, and the calcium content can reach about 19 to 20 percent.
However, there is no method for preparing a product with an ultra-high base number (TBN600), and those skilled in the art familiar with alkylbenzene sulfonate production know that the difficulty is higher when the product TBN is higher and the calcium content is higher in the process of preparing alkylbenzene sulfonate, calcium is easily removed in the production process, and the carbonation reaction fails due to the jelly. Therefore, how to prepare the ultra-high base number (TBN600) synthetic calcium alkyl benzene sulfonate becomes an urgent problem to be solved in the industry.
Disclosure of Invention
Aiming at the problems, the application provides a preparation method of the ultrahigh-base-number synthetic calcium alkyl benzene sulfonate, the method can prepare the ultrahigh-base-number synthetic calcium sulfonate with TBN600 and calcium content of about 22%, and the storage stability of the product diluted into base oil is good.
The preparation method of the ultrahigh-base-number synthetic calcium alkylbenzene sulfonate comprises the following steps:
adding sulfonic acid, diluent oil, a solvent and calcium oxide into a reaction bottle and uniformly mixing;
continuously adding an alcohol substance, dodecylphenol or calcium alkylphenol sulfide, an amine substance, calcium chloride and an acid substance into the reaction bottle, carrying out neutralization reaction at 45-55 ℃ for 30-90 minutes, and controlling the pH value in the reaction bottle to be 6-10 after the neutralization reaction is finished;
continuously adding calcium oxide, water and the alcohol substances into the reaction bottle for one time or multiple times, continuously introducing carbon dioxide into the reaction bottle for carbonation reaction, and controlling the temperature in the reaction bottle to be kept at 45-65 ℃ until the carbonation reaction is finished;
after the carbonation reaction is finished, heating the materials in the reaction bottle to 70-120 ℃, distilling out alcohol substances and water in the materials under the vacuum condition of 0-minus 0.09MPa, then removing residues by centrifugation, and further removing the solvent in the materials by reduced pressure distillation to obtain a finished product;
wherein the mass ratio of the sulfonic acid to the diluent oil is 65-110: 100, the mass ratio of the mixture formed by the sulfonic acid and the diluent oil, the solvent, the calcium oxide, the alcohol substance, the calcium dodecyl phenol or the calcium alkyl phenol sulfide, the amine substance, the calcium chloride, the acid substance and the water is
100：100-300：70-100：25-50：0-6：0-8：0-5：0-3：17-30。
Optionally, the sulfonic acid is one or a mixture of a heavy alkyl benzene sulfonic acid, a long chain linear alkyl benzene sulfonic acid.
Optionally, the alcohol substance is any one or combination of methanol, ethanol, propanol, isopropanol, n-butanol and isobutanol.
Optionally, the amine substance is any one or combination of ammonia, urea, amine carbonate, ethylenediamine, triethylenetetramine and tetraethylenepentamine.
Optionally, the acid substance is any one or more of formic acid, acetic acid, stearic acid, dodecahydroxystearic acid and boric acid.
Optionally, the solvent is an aromatic hydrocarbon solvent or an alkane solvent.
Optionally, the diluent oil is any one of non-hydrogenated oil, PAO, GTL.
The method comprises the steps of adding sulfonic acid, diluent oil, a solvent and calcium oxide into a reaction bottle and uniformly mixing; continuously adding an alcohol substance, dodecylphenol or calcium alkylphenol sulfide, an amine substance, calcium chloride and an acid substance into a reaction bottle, carrying out neutralization reaction at 45-55 ℃ for 30-90 minutes, and controlling the pH to be 6-10 after the reaction is finished; adding calcium oxide, water and alcohol substances at one time or multiple times, continuously introducing carbon dioxide for carbonation reaction, and controlling the temperature to be 45-65 ℃ until the carbonation reaction is finished; after the reaction is finished, the materials in the reaction bottle are heated to 70-120 ℃, alcohol substances and water in the materials are distilled out under the vacuum condition of 0-minus 0.09MPa, then the materials are centrifuged to remove residues, and the solvent in the materials is further removed by reduced pressure distillation to obtain the finished product. Thus, the synthesized calcium sulfonate with TBN600 and ultrahigh base number with calcium content of about 22 percent is prepared, and the storage stability of the product diluted into base oil is good.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
First embodiment
The preparation method of the ultrahigh-base-number synthetic calcium alkyl benzene sulfonate in the embodiment comprises the following steps of adding sulfonic acid, diluent oil, a solvent and calcium oxide into a reaction bottle and uniformly mixing; then continuing to add an alcohol substance, dodecylphenol or calcium alkylphenol sulfide, an amine substance, calcium chloride and an acid substance into the reaction bottle, carrying out neutralization reaction at 45-55 ℃ for 30-90 minutes, and controlling the final pH to be 6-10; and continuously adding calcium oxide, water and alcohol substances into the reaction bottle for one time or multiple times, continuously introducing carbon dioxide into the reaction bottle for carbonation reaction, and controlling the temperature in the reaction bottle to be kept at 45-65 ℃ until the carbonation reaction is finished.
After the carbonation reaction is finished, the materials in the reaction bottle are heated to 70-120 ℃, alcohol substances and water in the materials are distilled out under the vacuum condition of 0-minus 0.09MPa, then the materials are centrifuged to remove residues, and the solvent in the materials is further removed by reduced pressure distillation to obtain the finished product.
Wherein, the sulfonic acid can be one of heavy alkyl benzene sulfonic acid and long-chain linear alkyl benzene sulfonic acid or a mixture of the two in any proportion. The alcohol substance can be any one or combination of methanol, ethanol, propanol, isopropanol, n-butanol and isobutanol. The amine substance can be any one or combination of more of ammonia water, urea, amine carbonate, ethylenediamine, triethylenetetramine and tetraethylenepentamine. The acid substance can be any one or combination of more of formic acid, acetic acid, stearic acid, dodecahydroxystearic acid and boric acid. The mass ratio of the sulfonic acid to the diluent oil is 65-110: 100, the mass ratio of the mixture of sulfonic acid and diluent oil, solvent, calcium oxide, alcohol substance, calcium dodecylphenol or sulfurized alkylphenol, amine substance, calcium chloride, acid substance, water and carbon dioxide is
100：100-300：70-100：25-50：0-6：0-8：0-5：0-3：17-30：45-70。
Specifically, the sulfonic acid in this example is a mixture of a heavy alkylbenzene sulfonic acid and a long chain linear alkylbenzene sulfonic acid; the solvent consists of alkane with the distillation range of 150-190 ℃ and arene with the distillation range of 110-120 ℃, wherein the mass fraction of the alkane is 60 percent, and the mass fraction of the arene is 40 percent; the alcohol substance is composed of n-butanol and methanol; the acid substance is boric acid.
During preparation, firstly, 10g of heavy alkylbenzene sulfonic acid, 30g of long-chain linear alkylbenzene sulfonic acid, 60g of diluent oil, 100g of solvent and 3.5 g of calcium oxide are added into a reaction bottle and uniformly mixed, and then 12g of n-butyl alcohol, 30g of methanol, 6g of dodecylphenol, 0.8g of calcium chloride and 2g of boric acid are continuously added, so that the substances are subjected to neutralization reaction for 45 minutes at the temperature of 53-55 ℃, and the final pH is controlled to be 6-10; then the remaining 78g of calcium oxide and 26g of water were added to the reaction flask in 6 portions, and 57g of carbon dioxide was introduced into the reaction flask at a constant rate of 10 g/hr. The temperature of the materials is required to be kept between 53 and 55 ℃ in the whole process until the carbonation reaction is finished; and finally, heating the materials in the reaction bottle to 120 ℃, distilling out alcohol substances and water in the materials under the vacuum condition of 0-minus 0.09MPa, then centrifuging to remove residues, and further carrying out reduced pressure distillation to remove the solvent in the materials to obtain the finished product.
The base number of the product prepared by the process is 603mgKOH/g, the calcium content of the product reaches 22.15 percent, and the kinematic viscosity at 100 ℃ is 348mm2The turbidity of the product is 30NTU, the infrared spectrum detection shows that the product has a characteristic peak at 861cm (-1), and the calcium carbonate is in an amorphous state. 10g of the product is dissolved in 90g of 150BS base oil and kept at a constant temperature of 100 ℃ for 90 days, and an oil sample is clear, has no turbidity and no precipitate.
Second embodiment
The sulfonic acid in this example is a mixture of a heavy alkylbenzene sulfonic acid and a long chain linear alkylbenzene sulfonic acid; the diluent oil is 150SN diluent oil; the solvent consists of alkane with the distillation range of 150-190 ℃ and arene with the distillation range of 110-120 ℃, wherein the mass fraction of the alkane is 60 percent, and the mass fraction of the arene is 40 percent; the alcohol substance consists of isobutyl alcohol and methanol; the amine substance is amine carbonate; the acid substance is boric acid.
During preparation, firstly, adding 8g of heavy alkylbenzene sulfonic acid, 42g of long-chain linear alkylbenzene sulfonic acid, 50g of 150SN diluent oil, 170g of solvent and 3.0 g of calcium oxide into a reaction bottle, uniformly mixing, then continuously adding 15g of methanol, 15g of isobutanol, 5g of TBN260 calcium alkylphenol sulfide, 3g of amine carbonate and 2g of boric acid, and carrying out neutralization reaction on the substances at the temperature of 48-55 ℃ for 30 minutes, wherein the final pH is controlled to be 6-10; the remaining 81g of calcium oxide and 17.5g of water were then added to the reaction flask 7 times and 56g of carbon dioxide were passed through at a constant rate of 11 g/h. The temperature of the materials is required to be controlled to be kept between 53 and 55 ℃ in the whole process until the carbonation reaction is finished; and finally, heating the materials in the reaction bottle to 120 ℃, distilling out alcohol substances and water in the materials under the vacuum condition of 0-minus 0.09MPa, then centrifuging to remove residues, and further carrying out reduced pressure distillation to remove the solvent in the materials to obtain the finished product.
The product prepared by the above process has base number of 615mgKOH/g, calcium content of 22.6%, and kinematic viscosity of 268mm at 100 deg.C2The turbidity of the product is 25NTU, the infrared spectrum detection shows that the product has a characteristic peak at 861cm (-1), and the calcium carbonate is in an amorphous state. 10g of the product is dissolved in 90g of 150BS base oil and kept at a constant temperature of 100 ℃ for 90 days, and an oil sample is clear, has no turbidity and no precipitate.
Third embodiment
The sulfonic acid in this example is a mixture of a heavy alkylbenzene sulfonic acid and a long chain linear alkylbenzene sulfonic acid; the diluent oil is 150SN diluent oil; the solvent consists of alkane with the distillation range of 150-190 ℃ and arene with the distillation range of 110-120 ℃, wherein the mass fraction of the alkane is 60 percent, and the mass fraction of the arene is 40 percent; the alcohol substance consists of isopropanol and methanol; the amine substance consists of triethylene tetramine and amine carbonate; the acid substance is boric acid.
When in preparation, firstly, 25g of heavy alkylbenzene sulfonic acid, 27g of long-chain linear alkylbenzene sulfonic acid, 48g of 150SN diluent oil, 150g of solvent and 4.0 g of calcium oxide are added into a reaction bottle and evenly mixed; then, continuously adding 12g of methanol, 18g of isopropanol, 0.5g of triethylene tetramine, 5g of TBN150 calcium alkylphenol sulfide, 3g of amine carbonate and 0.5g of calcium chloride, carrying out neutralization reaction on the substances at the temperature of 48-55 ℃ for 30 minutes, and controlling the final pH to be 6-10; the remaining 81g of calcium oxide and 18g of water were then added to the reaction flask in 6 portions and 56g of carbon dioxide were passed through at a constant rate of 8 g/h. Maintaining the temperature of the whole process control at 53-55 deg.C until the end of the carbonation reaction; and finally, heating the materials in the reaction bottle to 120 ℃, distilling out the alcohols and the water in the materials under the vacuum condition of 0-minus 0.09MPa, then, centrifugally removing residues, and further carrying out reduced pressure distillation to remove the solvent in the materials to obtain the finished product.
The product prepared by the above process has base number of 605mgKOH/g, calcium content of 22.31%, and kinematic viscosity of 308mm at 100 deg.C2The turbidity of the product is 22NTU, the infrared spectrum detection shows that the product has a characteristic peak at 861cm (-1), and the calcium carbonate is in an amorphous state. 10g of the product is dissolved in 90g of 150BS base oil and kept at a constant temperature of 100 ℃ for 90 days, and an oil sample is clear, has no turbidity and no precipitate.
Fourth embodiment
The sulfonic acid in this example is a mixture of a heavy alkylbenzene sulfonic acid and a long chain linear alkylbenzene sulfonic acid; the diluent oil is 150N diluent oil; the solvent consists of alkane with the distillation range of 150-190 ℃ and arene with the distillation range of 110-120 ℃, wherein the mass fraction of the alkane is 60 percent, and the mass fraction of the arene is 40 percent; the alcohol substance consists of methanol and isobutanol; the amine substance consists of ethylenediamine and amine carbonate; the acid substance is boric acid.
When in preparation, firstly, 15g of heavy alkylbenzene sulfonic acid, 30g of long-chain linear alkylbenzene sulfonic acid, 55g of 150N diluent oil, 120g of solvent and 4.0 g of calcium oxide are added into a reaction bottle and evenly mixed; then, continuously adding 25g of methanol, 0.5g of ethylenediamine, 3g of TBN150 calcium alkylphenol sulfide, 2g of amine carbonate and 0.5g of boric acid, carrying out neutralization reaction on the substances at the temperature of 48-55 ℃ for 30 minutes, and controlling the final pH to be 6-10; the remaining 75g of calcium oxide, 24g of water and 15g of isobutanol were then added to the reaction flask 5 times and 56g of carbon dioxide was passed through at a constant rate of 8 g/h. Controlling the temperature of the materials to be kept at 53-55 ℃ in the whole process until the carbonation reaction is finished; finally, heating the materials in the reaction bottle to 120 ℃, distilling out alcohol substances and water in the materials under the vacuum condition of 0-minus 0.09MPa, then centrifuging to remove residues, and further carrying out reduced pressure distillation to remove the solvent in the materials to obtain a finished product;
the product prepared by the above process has a base number of 608mgKOH/g, a calcium content of 22.35%, and a kinematic viscosity of 246mm at 100 deg.C2The turbidity of the product is 29NTU, the infrared spectrum detection shows that the product has a characteristic peak at 861cm (-1), and the calcium carbonate is in an amorphous state. 10g of the product is dissolved in 90g of 150BS base oil and kept at a constant temperature of 100 ℃ for 90 days, and an oil sample is clear, has no turbidity and no precipitate.
The method comprises the steps of adding sulfonic acid, diluent oil, a solvent and calcium oxide into a reaction bottle and uniformly mixing; continuously adding an alcohol substance, dodecylphenol or calcium alkylphenol sulfide, an amine substance, calcium chloride and an acid substance into a reaction bottle, carrying out neutralization reaction at 45-55 ℃ for 30-90 minutes, and controlling the pH to be 6-10 after the reaction is finished; adding calcium oxide, water and alcohol substances at one time or multiple times, continuously introducing carbon dioxide for carbonation reaction, and controlling the temperature to be 45-65 ℃ until the carbonation reaction is finished; after the reaction is finished, the materials in the reaction bottle are heated to 70-120 ℃, alcohol substances and water in the materials are distilled out under the vacuum condition of 0-minus 0.09MPa, then the materials are centrifuged to remove residues, and the solvent in the materials is further removed by reduced pressure distillation to obtain the finished product. Thus, the synthesized calcium sulfonate with TBN600 and ultrahigh base number with calcium content of about 22 percent is prepared, and the storage stability of the product diluted into base oil is good.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal 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 terminal apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or terminal that comprises the element.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A preparation method of calcium alkyl benzene sulfonate synthesized by ultrahigh base number is characterized by comprising the following steps:
adding sulfonic acid, diluent oil, a solvent and calcium oxide into a reaction bottle and uniformly mixing;
continuously adding an alcohol substance, dodecylphenol or calcium alkylphenol sulfide, an amine substance, calcium chloride and an acid substance into the reaction bottle, carrying out neutralization reaction at 45-55 ℃ for 30-90 minutes, and controlling the pH value in the reaction bottle to be 6-10 after the neutralization reaction is finished;
continuously adding calcium oxide, water and the alcohol substances into the reaction bottle for one time or multiple times, continuously introducing carbon dioxide into the reaction bottle for carbonation reaction, and controlling the temperature in the reaction bottle to be kept at 45-65 ℃ until the carbonation reaction is finished;
after the carbonation reaction is finished, heating the materials in the reaction bottle to 70-120 ℃, distilling out alcohol substances and water in the materials under the vacuum condition of 0-minus 0.09MPa, then removing residues by centrifugation, and further removing the solvent in the materials by reduced pressure distillation to obtain a finished product;
wherein the mass ratio of the sulfonic acid to the diluent oil is 65-110: 100, the mass ratio of the mixture formed by the sulfonic acid and the diluent oil, the solvent, the calcium oxide, the alcohol substance, the calcium dodecyl phenol or the calcium alkyl phenol sulfide, the amine substance, the calcium chloride, the acid substance and the water is
100：100-300：70-100：25-50：0-6：0-8：0-5：0-3：17-30；
Wherein the sulfonic acid is one or a mixture of heavy alkylbenzene sulfonic acid and long-chain linear alkylbenzene sulfonic acid;
wherein the alcohol substance is any one or combination of more of methanol, ethanol, propanol, n-butanol and isobutanol;
wherein the amine substance is any one or combination of more of ammonia water, urea, ammonium carbonate, ethylenediamine, triethylene tetramine and tetraethylene pentamine;
wherein, the acid substance is any one or combination of more of formic acid, acetic acid, stearic acid, dodecahydroxystearic acid and boric acid;
wherein the solvent is an aromatic hydrocarbon solvent or an alkane solvent;
wherein the diluent oil is non-hydrogenated oil or hydrogenated oil.
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|---|---|
| CN108017563A (en) | 2018-05-11 |
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