CN103694147B - A kind of preparation method of sulfonate detergent - Google Patents
A kind of preparation method of sulfonate detergent Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of sulfonate detergent; First by sulfonic acid or sulfonic acid normal salt, the metal oxide of 5～40 weight portions or the metal hydroxides of 20～160 weight portions of flux oil 100 weight portions containing 40～60% weight, the promoter raw material of 5～100 weight portions mixes, within 15～65 DEG C, carry out metallization reaction, middle and high or overbased sulfonate need lead to the carbon dioxide of 10～70 parts; Then, temperature of charge is risen to 65～100 DEG C, steam the promoter of removing wherein, the material that contains water, under the condition that is less than 100 DEG C, is continued to reaction at least 1 hour, last, then continue intensification flash distillation, steam and dewater and solvent; Promoter is one or more the mixture of carboxylic acid, organic amine, phenol, hydroxyl thing of low-carbon alcohols, water, the C1 to C7 of C1 to C8; This preparation method's yield is high, and constant product quality, especially suitability for mass industrialized application of installation.
Description
Technical field
The present invention relates to a kind of preparation method of sulfonate, especially a kind of system of sulfonate detergentPreparation Method, belongs to oil dope field.
Background technology
Oil-soluble sulfonic acid salt has good solubilising, dispersion, washing, the function such as antirust, to startingMachine surface has extremely excellent peace and quiet effect, adds with the oil product such as ashless dispersant, oxidation and corrosion inhibitorThe compound property that adds agent is good, is widely used in vapour, Diesel engine and makes as detergent for lubricating oilWith.
According to total base number or tenor, serial sulfonate product mainly contain low alkali value sulfonate, inThe even overbased sulfonate of base number sulfonate, over base sulfosalt; According to metal species, seriesSulfonate product mainly contains potassium, sodium, calcium, magnesium, barium salt, or the compounded sulfonate of these metals.
Sulfonate is generally by the sulfonic acid or sulfonic acid normal salt and alkali or the alkaline-earth metal chemical combination that contain flux oilThing comes through technical process such as metallization reaction and post processing separation under solvent, promoter existPreparation. As U.S4,615,841, U.S4,617,135, U.S5,108,630, CN1231283,CN1990465 philosophy discloses low alkali value sulfoacid calcium, overbased sulfonic acid magnesium, overbased sulphurThe preparation method of acid calcium, high base number composition metal sulfonate.
Prepare sulfonate and mainly comprise four parts, be i.e. reactive moieties, expansion drying part, slagging-offFF and solvent recovery part. Concrete preparation process is: first, will contain the sulphur of flux oilThe oxide of acid or sulfonic acid normal salt, alkali or alkaline-earth metal or hydroxide, solvent, promoter (asMethyl alcohol etc.) etc. reactant mix, in reaction system, carry out low alkalization, cross the metal such as alkalizationChange reaction, then, will contain the material of solvent, water (comprising the water that reaction generates) and promoterThe flash distillation that heats up, air lift is dry, steams whole promoter, water and solvent, last, more logicalThe modes such as centrifugal or filtration of crossing remove the gred to refine and can prepare serial sulfonate detergent product.Wherein methyl alcohol is the primary accelerator of the preparation series sulfonate detergent of generally acknowledging.
In the preparation process of sulfonate, generally all wish quick expansion drying, especially on large ruleIn mould production process, steam fast after metallization reaction promoter, water and large in material in order to reachThe object of partial solvent, generally all adopts U.S4,615,841 disclosed external circulation heating flash distillation modesThe flash distillation that heats up, production procedure is according to schematic diagram 1. The temperature one of external circulation heating flash systemAs be controlled at more than 100 ± 2 DEG C, the solvent with rapid steaming except promoter, water and part.
The disposable essence that is rapidly heated flash distillation mode is to steam fast after metallization reaction in materialMethyl alcohol primary accelerator and water. After metallization reaction finishes, the quality of the sulfonate micelle in material is notVery stable, the mode of this disposable flash distillation that is rapidly heated not only to a certain degree affects final productsQuality, especially causes in thick product solid content higher, and metallization efficiency and synthesis yield are lower.
Summary of the invention
The preparation method who the invention provides a kind of sulfonate detergent, utilizes the method, not only canPrepare the stable serial sulfonate detergent product of low turbidity, and in thick product, solid content is low,Synthesis yield is high, especially suitability for mass industrialized application of installation.
Concrete sulfonate preparation process of the present invention is: first, and by the sulfonic acid of 100 weight portions or sulphurThe metal oxide or 20～160 of acid normal salt (containing 40～60% flux oil), 5～40 weight portionsThe metal hydroxides of weight portion, the promoter raw material of 5～100 parts mixes, 15～65Within DEG C, carry out metallization reaction at the reaction system with heating function, (middle and high or superelevation alkaliValue sulfonate need lead to the carbon dioxide of 10～70 weight portions), then, will contain promoter and waterMaterial carries out temperature-gradient method, and expansion drying finally removes the gred refining, can prepare outward appearance saturatingSerial sulfonate detergent product bright, oily.
Sulfonic acid of the present invention refers to mahogany acid (sulfonic group is on aromatic ring or naphthenic ring); Alkyl virtueBase sulfonic acid (sulfonic group is on aromatic ring); Alkyl and olefin sulfonic acid; Polyoxyethylene ether sulfonic acid (sulfonic acidBase is at the oxygen ethyl end of the chain) or polycyclic aromatic hydrocarbon sulfonate condensation product (sulfonic group is on aromatic ring) etc., mainRefer to be replaced by alkyl, particularly from petroleum distillate, alkylating aromatic hydrocarbon is synthetic or both are mixedThe mahogany acid, alkyl benzene sulphonate or the mixing sulfonic acid that close the aromatic hydrocarbons of the alkyl replacement obtaining and obtain.Different according to source, the aromatic ring part that preferred each alkyl replaces contains 16 to 80 carbon atoms of having an appointment,More preferably 18 to 40 carbon atoms.
Alkali of the present invention or alkaline earth metal compound are mainly oxide or the hydrogen-oxygens of alkali or alkaline-earth metalCompound, if master metal lithium, sodium, potassium, magnesium, calcium, barium etc. are concrete as lithium hydroxide, hydrogen-oxygenHua Na ﹑ potassium hydroxide, Qing Yangization Gai ﹑ Yangization Gai ﹑ Yangization Mei ﹑ barium hydroxide etc., preferably hydrogen-oxygenChange lithium, Qing Yangization Na ﹑ Qing Yangization Gai ﹑ calcium oxide or magnesia, more preferably Qing Yangization Gai ﹑ oxidationCalcium or magnesia.
The present invention can use the solvent of 20～200 parts, or does not use solvent. Select low viscousAlkane, aromatic hydrocarbons, alcohol or its mixture make solvent, as alkane, the C6 to C10 of C3 to C10Aromatic hydrocarbons, alcohol or its mixture etc. of C3 to C8, concrete as heptane, isooctane, benzene, alkylBenzene,toluene,xylene, n-butanol etc.
Promoter of the present invention be selected from low-carbon alcohols, water, the C1 to C7 of C1 to C8 carboxylic acid, haveMachine amine, phenol, hydroxyl thing etc. can be also two or more mixtures wherein. Methyl alcoholIt is generally acknowledged primary accelerator
Metallization reaction of the present invention mainly refers to low alkalization or/and cross quaternization. Low basifier is generalBe exactly alkali or alkaline earth metal compound, the oxide of preferred bases or alkaline-earth metal or hydroxide. CrossBasifier is generally carbon dioxide, boron source (as boric acid etc.), sulfur dioxide or its mixture etc., excellentThe basifier excessively of choosing is carbon dioxide.
Metallization reaction temperature of the present invention is 15～65 DEG C, preferably 25～60 DEG C. Metallization is anti-Answer pressure under atmospheric pressure, exceed or lower than carrying out under the pressure of atmosphere, preferably at atmospheric pressureUnder carry out metallization reaction.
The described reaction system with heating function refer to there is interior circulating-heating, reacting kettle jacketing addsThe reaction system of hot or interior other pipe heating function, or there is two or more Hybrid HeatingThe reaction system of function.
Temperature-gradient method of the present invention refers to: after metallization reaction finishes, first temperature of charge is risen to65～100 DEG C, steam the primary accelerator methyl alcohol removing wherein, then, will contain water and (comprise metallization anti-The water that should generate) material under the condition that is less than 100 DEG C, continue reaction at least 1 hour,After, then continue intensification flash distillation, steam and dewater and solvent etc.
Expansion drying of the present invention refers to and steams except whole component such as solvent, water in system, until waterPart is less than 0.5%. Select air lift mode.
That slagging-off of the present invention adopts is centrifugal, sedimentation or filter type. In embodiment, adopt filter typeSlagging-off.
In preparation method of the present invention, the mixed material obtaining after temperature-gradient method, selects first to dodgeEvaporate to dryness is dry, then removes the gred, or first removes the gred, and then carries out expansion drying. The present invention is excellentSelect first expansion drying, the post processing separation and purification mode then removing the gred.
The material of the sulfonate that the present invention generates by the metallization reaction adopting containing methyl alcohol, waterThe mode of temperature-gradient method, the stable serial sulfonate detergent that not only can prepare low turbidity producesProduct, and metallization efficiency is high, and synthesis yield is high, especially suitability for mass industrialized application of installation.
Brief description of the drawings
Fig. 1 has the reaction system schematic flow sheet of external circulation heating flash distillation function
Wherein: 1 reactor, 2 external circulation heaters, 3 flash tanks, 4 drying kettles, 5 is coldCondenser, 6 slag removing systems, 7 recycling cans, 8 deodorizing systems, 9 liquid recovery systems.
Fig. 2 has the reaction system schematic flow sheet of interior circulating-heating flash distillation function
Wherein: 1 reactor, 2 flash tanks, 3 interior recirculation heaters, 4 condensers,5 slag removing systems, 6 recycling cans, 7 deodorizing systems, 8 liquid recovery systems.
Detailed description of the invention
Indices analytical method in the embodiment of the present invention:
1. total base number SH/T0251
2. calcium content SH/T0297
3. viscosity GB/T265
4. turbidity SH/T0028
Embodiment 1
Production procedure is shown in that accompanying drawing 2 shows. The process units of low alkali value sulfonate detergent is by metallization reactionThe refining two part compositions of part and post processing; Comprise reactor 1, flash tank 2, interior recirculation heater3, condenser 4, slag removing system 5, recycling can 6, deodorizing system 7; Slag tap in reactor 1 bottomMouth is connected with slag removing system 5 by pipeline; Reactor 1 top exit is by pipeline and flash tank 2The charging aperture that is positioned at bottom connects; Flash tank 2 is positioned at the outlet at top by condenser 4 and recoveryTank 6 connects, and the water out that is positioned at recycling can 6 bottoms is connected with charging system 8 by pump; Be positioned atThe outlet at recycling can 6 tops is connected with deodorizing system 7 by pipeline; Flash tank 2 is positioned at topAnother outlet is connected with slag removing system 5 by interior recirculation heater 3.
Under normal temperature, successively to 53 cubic meter bands stir reactor in add 26909Kg neutral oil,2840Kg water, 3558Kg white lime (industrial goods, purity 95%), 15791Kg heavy alkyl benzene sulphurAcid (Jinzhou company industrial goods, directly acid number 132.5mgKOH/g), opens reactor simultaneously and stirs(and/or circulating pump), by even mixing of materials in still, still temperature show value is 60 DEG C, isothermal reactionApproximately 3 hours. Then, material in reactor is warming up to 90 DEG C, constant temperature stirred after 1 hour, continuedContinue and be warming up to 145～155 DEG C,, flow with 100Kg/h by the gas distribution tube of Polycondensation Reactor and Esterification Reactor meanwhileSpeed passes into dry air, until the moisture analysis value in material is 0.12%, stops logical dry air,Recording thick product solid content is 2.8%(m/m).
In the moisture content material of qualified (being less than 0.5%), add 2000Kg super-cell (JiLin Changbai), mix and pass through filtration system filters, last, add the punching of 6000Kg neutral oilWash system, flushing filtering system obtains about 48750Kg low alkali value calcium alkylbenzenesulfonate industrial goods. Through meterCalculate yield (hundred of product weight centering oil, sulfonic acid, three kinds of effective raw material gross weights of white limeProportion by subtraction) be 93.3%.
Industrial products test result is total base number 29.4mgKOH/g, calcium content 2.85%, turbidity4JTU, viscosity 15.7mm2/s。
Comparative example 1
Production procedure is shown in that accompanying drawing 1 shows. Comprise reactor 1, flash tank 2, external circulation heater 3,Condenser 4, slag removing system 5, recycling can 6, deodorizing system 7; Reactor 1 outlet at bottom passes throughPipeline is connected with external circulation heater 3; External circulation heater 3 is positioned at entering of top with flash tank 2Material mouthful connects; The outlet that flash tank 2 is positioned at top is connected with recycling can 6 by condenser 4, positionWater out in recycling can 6 bottoms is connected with charging system 8 by pump; Be positioned at recycling can 6 topsOutlet be connected with deodorizing system 7 by pipeline; Flash tank 2 is positioned at the outlet of bottom and passes through pipelineThe entrance that is positioned at top with drying kettle 9 is connected, and is positioned at outlet and the slag removing system of drying kettle 9 bottoms5 connect.
Under normal temperature, successively to 53 cubic meter bands stir reactor 1 in add 26909Kg neutral oil,1858Kg calcium chloride water (concentration 4.72%%), 1200Kg n-butanol, 1085Kg methyl alcohol,3720Kg white lime (industrial goods, purity 95%), 14800Kg heavy alkylbenzene sulfonic acid (Jinzhou public affairsDepartment's industrial goods, directly acid number 132.5mgKOH/g), be naturally warming up to 60 DEG C, isothermal reaction approximately 3Hour.
Get through external circulation heating system flow, and the temperature of controlling external circulation heater 2 is 104 ± 2DEG C, liquid material is poured in drying kettle 4 in quick flash distillation, and drying kettle receives liquid materialTime continue intensification flash distillation; Batch turning finishes, and still temperature rise to 118 DEG C, by the gas at the bottom of drying kettleBody distributor pipe passes into dry air with 100Kg/h flow velocity, until material moisture content assay value is 0.23%,Stop logical dry air, recording thick product solid content is 12.4%(m/m), and material is poured into and removedSlag system.
At slag removing system, in the moisture content material of qualified (being less than 0.5%), add 8250Kg diatomSoil filter aid (Changbai), by filtration system filters, last, obtain the low alkali of 19040KgValue calcium alkylbenzenesulfonate industrial goods. As calculated, yield (product weight centering oil, sulfonic acid, ripe stoneThe percentage of three kinds of effective raw material gross weights of ash) be 41.9%.
Industrial products test result is total base number 19.4mgKOH/g, calcium content 1.91%, turbidity68JTU, viscosity 36.4mm2/s。
Embodiment 2
Under normal temperature, in the there-necked flask of 2L belt stirrer, add 200g toluene (Jinzhou public affairs successivelyDepartment's industrial goods), 120g neutral oil, 22g methanol aqueous solution (methanol content 47.5%), 55g oxygenChange magnesium (industrial goods, purity 95.2%), 23g ammonium formate solution, 80g heavy alkylbenzene sulfonic acid (brocadeState company industrial goods, directly acid number 121.8mgKOH/g), stir, the temperature rise of material nature is extremely58 DEG C. Then, control under the condition of temperature of charge≤60 DEG C, by inserting there-necked flask bottomGas distribution tube passes into carbon dioxide with 300ml/min speed, after 2 hours 20 minutes, stops twoCarbonoxide.
Utilize the electric heating cover heating of there-necked flask outside, after 7 minutes, material is warming up to 72 DEG C,And steam the methyl alcohol in system, under 75 ± 5 DEG C of conditions, constant temperature stirs 1 hour. Then, continueThe continuous electric heating cover that utilizes heats, and after 23 minutes, temperature of charge rises to 120 DEG C, passes through distribution of gasPipe passes into dry air with 300ml/min flow velocity, rises to 150 DEG C of left and right, freeze-day with constant temperature half an hour,Stop expansion drying. Recording thick product solid content is 2.0%(m/m), last, in material, addEnter 20g super-cell (Changbai), mix, filter, obtain about 280.2g superHigh base number synthesizes sulfonic acid magnesium product.
As calculated, yield (four kinds of product weight centering oil, sulfonic acid, magnesia, carbon dioxideThe effectively percentage of raw material gross weight) be 83.0%.
Product test result is total base number 438mgKOH/g, content of magnesium 9.38%, and turbidity 23JTU,Viscosity 106.7mm2/s。
Comparative example 2
Under normal temperature, in the there-necked flask of 2L belt stirrer, add 200g toluene (Jinzhou public affairs successivelyDepartment's industrial goods), 120g neutral oil, 22g methanol aqueous solution (methanol content 47.5%), 55g oxygenChange magnesium (industrial goods, purity 95.2%), 23g ammonium formate solution, 80g heavy alkylbenzene sulfonic acid (brocadeState company industrial goods, directly acid number 121.8mgKOH/g), stir, the temperature rise of material nature is extremely58 DEG C. Then, control under the condition of temperature of charge≤60 DEG C, by inserting there-necked flask bottomGas distribution tube passes into carbon dioxide with 300ml/min speed, after 2 hours 30 minutes, stops twoCarbonoxide.
Utilize the electric heating cover heating of there-necked flask outside, after 27 minutes, temperature of charge rises to rapidly120 DEG C, pass into dry air by gas distribution tube with 300ml/min flow velocity, rise to 150 DEG C of left sidesThe right side, freeze-day with constant temperature half an hour, stops expansion drying. Recording thick product solid content is 9.2%(m/m),Finally, in material, add 30g super-cell (Changbai), mix, filter,Obtain about 235.3g Overbased magnesium sulphonates product.
As calculated, yield (four kinds of product weight centering oil, sulfonic acid, magnesia, carbon dioxideThe effectively percentage of raw material gross weight) be 68.5%.
Product test result is total base number 382mgKOH/g, content of magnesium 8.67%, and turbidity 268JTU,Viscosity 258.9mm2/s。
Embodiment 3
Under normal temperature, in the reactor 1 stirring to 53 cubic meter bands successively, add 19000Kg toluene (brocadeState company industrial goods), 10430Kg neutral oil, 5720Kg methanol aqueous solution (methanol content 47.5%),6000Kg magnesia (industrial goods, purity 95.2%), 2550Kg ammonium formate solution, 9045KgHeavy alkylbenzene sulfonic acid (Jinzhou company industrial goods, directly acid number 121.8mgKOH/g), by thing in stillMaterial mixes, and still temperature show value is 54 DEG C. Then, the gas distribution tube by Polycondensation Reactor and Esterification Reactor with200Kg/h speed passes into carbon dioxide, meanwhile, controls temperature of charge≤60 DEG C in reactor,After 35 hours 50 minutes, stop carbon dioxide. Then, the material in reactor is warming up to 76 DEG C,And steaming the methyl alcohol in system, constant temperature stirs 2 hours; While continuing to be warming up to 115 DEG C, by insteadAnswer the gas distribution tube at the bottom of still to pass into dry air with 100Kg/h flow velocity, until still temperature to 145～155 DEG C time, monitoring analysis material moisture content, is less than 0.5% and is until moisture analysis value is 0.18%(Qualified), stop logical dry air, recording thick product solid content is 3.2%(m/m), material is fallenEnter slag removing system.
In the qualified material of moisture content, add 2500Kg super-cell (Changbai), pass throughFiltration system filters, last, add 5000Kg neutral oil flushing filtering system, obtain approximately32080Kg Overbased magnesium sulphonates industrial goods. As calculated, yield (product weight centeringThe percentage of oil, sulfonic acid, magnesia, four kinds of effective raw material gross weights of carbon dioxide) be 85.2%.
Industrial products test result is total base number 427mgKOH/g, content of magnesium 9.58%, turbidity32JTU, viscosity 98.5mm2/s。
The synthetic effect data rows following table 1 of each embodiment is shown
Table 1 combined coefficient
In table 1, data show: the product base number of the inventive method is high, and turbidity is low, and viscosity is little, matterMeasure more stable; The thick product solid content of the inventive method is less than 4%, and synthesis yield reaches more than 80%,The good product quality of the inventive method is described, metallization efficiency and production efficiency are high, have substanceImprovement.
Claims (4)
1. a preparation method for sulfonate detergent, is characterized in that: first will be containing 40～The heavy alkylbenzene sulfonic acid of 100 weight portions of the flux oil of 60% weight, 5～40 weight portionsThe calcium hydroxide of magnesia or 20～160 weight portions, the promoter raw material of 5～100 weight portionsMix, at 15～65 DEG C, in the reaction system with cooling and heating function, carry outMetallization reaction, need pass into 10～70 weight portions while preparing middle and high or overbased sulfonateCarbon dioxide; Then, temperature of charge is risen to 65～100 DEG C, steams the promoter of removing wherein,The material that contains water, under the condition that is less than 100 DEG C, is continued to reaction at least 1 hour, last,Continue again intensification flash distillation, steam and dewater and solvent, and it is refining to remove the gred;
Described promoter be low-carbon alcohols, water, the C1 to C7 of C1 to C8 carboxylic acid, haveOne or more mixture of machine amine, phenol, hydroxyl thing;
Described method can add the solvent of 20～200 weight portions, or does not use solvent.
2. according to the preparation method of sulfonate detergent claimed in claim 1, its feature existsRefer to low alkalization or/and cross quaternization in: described metallization reaction, low basifier be alkali orAlkaline earth metal compound; Crossing basifier is carbon dioxide.
3. according to the preparation method of sulfonate detergent claimed in claim 1, its feature existsIn: described metallization reaction temperature is 25～60 DEG C; Metallization reaction pressure is at atmospheric pressureUnder power, exceed or lower than carrying out under the pressure of atmosphere.
4. according to the preparation method of sulfonate detergent claimed in claim 1, its feature existsRefer in: the described reaction system with heating function there is interior circulating-heating, reactor folderThe reaction system of cover heating or interior other pipe heating function, or there is the mixed of two or moreClose the reaction system of heating function.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107022397B (en) * | 2016-02-01 | 2020-04-21 | 江西福安路润滑材料有限公司 | Sulfonate detergent, and preparation method and application thereof |
| CN106187827B (en) * | 2016-07-13 | 2018-09-21 | 新乡市瑞丰新材料股份有限公司 | A kind of preparation method of sulfonate |
| CN112980539A (en) * | 2021-02-02 | 2021-06-18 | 安徽澳润新材料有限公司 | Chlorine-free high-base-number calcium sulfonate detergent and preparation method thereof |
| CN112899059A (en) * | 2021-02-25 | 2021-06-04 | 江苏澳润新材料有限公司 | Chlorine-free low-base-number calcium sulfonate detergent and preparation method thereof |
| CN115247089A (en) * | 2021-04-28 | 2022-10-28 | 中国石油天然气股份有限公司 | Preparation method of low-base-number alkylbenzene sulfonate |
| CN113831267A (en) * | 2021-09-08 | 2021-12-24 | 江苏澳润新材料有限公司 | Production process capable of improving purity of sulfonate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4615841A (en) * | 1983-09-22 | 1986-10-07 | Dresser Industries, Inc. | Process for making alkaline-earth metal salts of alkaryl sulfonic acids |
| US4617135A (en) * | 1985-04-11 | 1986-10-14 | Witco Corporation | Process for the preparation of overbased magnesium sulfonates |
| US5108630A (en) * | 1990-10-10 | 1992-04-28 | Texaco Inc. | Process for overbasing sulfonates comprising two separate additions of calcium oxide |
| CN1231283A (en) * | 1998-04-03 | 1999-10-13 | 中国石油化工总公司 | Process for preparing high basicity double-metal compounded sulfonate |
| CN1990463A (en) * | 2005-12-27 | 2007-07-04 | 中国石油化工股份有限公司 | High basicity mahogany sulfonate and its preparation method |
-
2012
- 2012-09-28 CN CN201210367655.3A patent/CN103694147B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4615841A (en) * | 1983-09-22 | 1986-10-07 | Dresser Industries, Inc. | Process for making alkaline-earth metal salts of alkaryl sulfonic acids |
| US4617135A (en) * | 1985-04-11 | 1986-10-14 | Witco Corporation | Process for the preparation of overbased magnesium sulfonates |
| US5108630A (en) * | 1990-10-10 | 1992-04-28 | Texaco Inc. | Process for overbasing sulfonates comprising two separate additions of calcium oxide |
| CN1231283A (en) * | 1998-04-03 | 1999-10-13 | 中国石油化工总公司 | Process for preparing high basicity double-metal compounded sulfonate |
| CN1990463A (en) * | 2005-12-27 | 2007-07-04 | 中国石油化工股份有限公司 | High basicity mahogany sulfonate and its preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 曲江.高碱值烷基苯磺酸钙合成工艺研究.《石油炼制与化工》.2009,第40卷(第10期),46-50页. * |
| 裴宏斌和曲江.超高碱值合成磺酸镁的研制与生产.《辽宁化工》.2004,第33卷(第10期),568-570页. * |
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