CN100584443C - SO3 gas jetting sulfonation reactor and process - Google Patents
SO3 gas jetting sulfonation reactor and process Download PDFInfo
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Abstract
The SO3 gas jetting sulfonation reactor consists of a nozzle and a reactor kettle. The nozzle includes a gas jet, a liquid distributing cavity, an atomizing jet, a liquid material inlet and a gas mixture inlet. The nozzle is fixed in the top of the reactor kettle, the atomizing jet is stretched into inside of the reactor kettle, and the reactor kettle has product outlet in the lower end. The present invention is suitable for sulfonating different kinds of organic material, and has the advantages of reasonable structure, great operation flexibility, simple operation, easy material replacement, stable product quality, etc.
Description
Technical field
The present invention relates to a kind of equipment and technique for applying thereof for preparing anion surfactant with sulfur trioxide gas sulfonation organic matter.
Background technology
Surfactant industry is one of important composition of fine chemistry industry, and at home and abroad development is exceedingly fast in recent years, and sulfonating reaction is to produce the most important technology of anion surfactant.Industrial oleum commonly used, chlorosulfonic acid, sulfur trioxide gas are made sulfonating agent, produce alkylbenzenesulfonate (LAS), fatty alcohol/ether alcohol sulfate (AS/AES), alpha-alkene sulfonate (AOS), MES anion surfactants such as (MES).Wherein preceding two kinds of process for sulfonation are serious because of environmental pollution, spent acid can't processing, poor product quality is eliminated gradually.At present, both at home and abroad making sulfonating agent with sulfur trioxide gas, to produce the capital equipment of anion surfactant be film sulfonation reactor.All there are relevant patent of invention in Italy Ballestra, U.S. Chemithon, companies such as Italian Mazzoni, Japanese Lion.The pattern of film sulfonation reactor is similar to shell-and-tube heat exchanger, (or otherwise) forms film from top to bottom in reaction tube to liquid state organics through the slit, sulfur trioxide gas also passes through in reaction tube from top to bottom, and vigorous reaction takes place for the two, and reaction heat is removed by the cooling water of shell side.There is following shortcoming in this class sulphonator: (1) complex structure, and equipment processing, the accuracy of manufacture and installation accuracy are had relatively high expectations, and investment cost is big; (2) operating flexibility is little, and process conditions are strict, is not suitable for the situation of frequent start-stop car; (3) be not suitable for containing wax, be difficult for film forming, easily coking, be subjected to organic sulfonation such as thermo-responsive.For example: during with film sulfonator sulfonation of Heavy (accessory substance of alkylbenzene production process), the easy coking in film sulfonator top, with short production cycle, must often stop and clean.
The patent of invention for preparing anion surfactant with jet sulfonation reactor mainly contains U.S. Chemithon company (US 4113438,1978) and University Of Tianjin (CN 96107060,1996).The former is with organic matter and SO
3Gas is sent into Venturi throat simultaneously and is carried out Forced Mixing, and the latter is a liquid gas class injection circulation reactor of making medium with high speed liquid phase workmanship.The two weak point is: must repeatedly circulate to sulfonated products just to reach the purpose that improves conversion ratio.And the viscosity of sulfonated products (when especially carbochain is longer) is far above raw material, and viscosity sharply increases when high conversion, not only bad for circulation, spray, and easily causes side reactions such as oversulfonate, oxidation, influences product quality.
Summary of the invention
The SO 3 gas jetting formula sulfonation reactor and the technique for applying thereof that the purpose of this invention is to provide a kind of conversion ratio height, good product quality.
SO of the present invention
3The gas blowing type sulfonation reactor is by nozzle, the reactor kettle is formed, it is characterized in that nozzle comprises gas nozzle, the liquid distribution chamber, atomizing mouth, liquid phase feed inlet and mist inlet, gas nozzle communicates with the mist inlet and is fixed in top, liquid distribution chamber, the liquid phase feed inlet is positioned at the bottom of side, liquid distribution chamber, atomizing mouth is fixed in the liquid distribution chamber, the gas nozzle bottom enters in the atomizing mouth, the atomizing mouth top is an opening, the position of atomizing mouth top in the liquid distribution chamber is higher than the position of liquid phase feed inlet in the liquid distribution chamber, nozzle is fixed in reactor kettle top, the atomizing mouth bottom enters in the reactor kettle, and there is the product outlet reactor kettle lower end.
Aforesaid nozzle can evenly distribute with 2～60 on reactor kettle top.
Can also be fixed with guide shell in the aforesaid reactor kettle, the atomizing mouth bottom enters in the guide shell.
When carrying out sulfonating reaction, the organic matter that is sulfonated enters the liquid distribution chamber by the liquid phase feed inlet, enters atomizing mouth through the overflow of atomizing mouth top again, flows downward SO then along the atomizing mouth inwall
3/ air gas mixture enters gas nozzle, SO by the mist inlet
3/ air gas mixture sprays in the reactor kettle with the organic matter contact and from atomizing mouth reacts sulfonating reaction product that obtains and unreacted SO
3/ air gas mixture is discharged from the product outlet.
SO of the present invention
3The operating procedure that gas sprays process for sulfonation is as follows:
By the aerial concentration of volume percent of sulfur trioxide is 3～15%, is preferably in 6～12%, with SO
3/ air is mixed into mist also after filtering, and mist enters SO
3The gas nozzle of gas blowing type sulfonation reactor, SO during air inlet body nozzle
3/ air gas mixture temperature is between 55～70 ℃, and in 50m/s～300m/s scope, organic matter enters SO from the gas speed of gas nozzle ejection
3Temperature during the gas blowing type sulfonation reactor is controlled between 5 ℃～100 ℃, organic matter and SO
3Mol ratio be controlled at 1.0～2.0: between 1, organic matter and SO
3/ air gas mixture is at SO
3React 1～5 second reaction time in the reactor kettle, sulfonating reaction product and unreacted SO in the gas blowing type sulfonation reactor
3/ air gas mixture is from SO
3After the product outlet of gas blowing type sulfonation reactor is discharged, carry out gas-liquid separation, liquid phase is after cooling, continue reaction 10～90min down at 10～80 ℃, the water that under agitation adds sulfonic acid weight 0～1.5% then, 10～80 ℃ of following hydrolysis 0～90 minute, be neutralized to pH6～9 with aqueous slkali and promptly obtain finished product.
Aforesaid unreacted SO
3/ air gas mixture can recycle.
Aforesaid SO
3Be by combustion sulphur method, oleum acid gas formulation or liquid SO
3The evaporation preparation.
Aforesaid organic matter is the alkylbenzene of alkane chain carbon number between 0～20, Fluhyzon, alkyl diphenyl ether, alkane chain carbon number at 8～20 fatty alcohol, AEO, APES.
Aforesaid alkali is organic bases such as inorganic bases such as NaOH, potassium hydroxide, ammonium hydroxide, magnesium hydroxide, calcium hydroxide and MEA, diethanol amine, triethanolamine, tetraalkylammonium hydroxide.
Compare SO of the present invention with existing film sulfonation reactor and technology
3Gas blowing type sulfonation reactor and technology have the following advantages:
(1) is applicable to the multiple Organic Ingredients of sulfonation, not only comprises all raw materials that are applicable to membrane-type sulfonation technology, and comprise the high viscosity that is not suitable for membrane-type sulfonation technology, contain wax, difficult film forming, thermal sensitivity Organic Ingredients.
(2) jet sulfonation reactor is rational in infrastructure, and operating flexibility is big and easy, and maintenance cost is low, and the raw material easy switching is adapted to the production model of the many kinds of small lot, also can satisfy the requirement of the big production of scale simultaneously.
(3) with the sulfur trioxide gas be working media, once spray and to reach required conversion ratio, do not adopt the mode of the sulfonated products that repeatedly circulates, constant product quality.
Description of drawings
Fig. 1 is a structural representation of the present invention
As shown in the figure, the 1st, liquid phase feed inlet, the 2nd, mist inlet, the 3rd, gas nozzle, the 4th, liquid distribution chamber, the 5th, atomizing mouth, the 6th, guide shell, the 7th, reactor kettle, the 8th, product outlet.
The specific embodiment
Embodiment 1: the sulfonation of detergent alkylate
SO
3The gas blowing type sulfonation reactor is by nozzle, the reactor kettle is formed, nozzle is by gas nozzle 3, liquid distribution chamber 4, atomizing mouth 5, liquid phase feed inlet 1 and mist inlet 2 are formed, gas nozzle 3 communicates with mist inlet 2 and is fixed in 4 tops, liquid distribution chamber, liquid phase feed inlet 1 is positioned at the bottom of 4 sides, liquid distribution chamber, atomizing mouth 5 is fixed in the liquid distribution chamber 4, gas nozzle 3 bottoms enter in the atomizing mouth 5, atomizing mouth 5 tops are openings, the position of atomizing mouth 5 tops in liquid distribution chamber 4 is higher than the position of liquid phase feed inlet 1 in liquid distribution chamber 4, nozzle is fixed in reactor kettle 7 tops, atomizing mouth 5 bottoms enter in the reactor kettle 7, and there is product outlet 8 reactor kettle 7 lower ends.
The industry alkylbenzene (average molar mass: 240) under 25 ℃ with the flow velocity of 15kg/h continuously by SO
3The liquid phase inlet 1 of gas blowing type sulfonation reactor enters liquid distribution chamber 4, enters atomizing mouth 5 through atomizing mouth 5 top overflows again, flows downward SO along atomizing mouth 5 inwalls then
3/ air (volume ratio 12%) mist enters gas nozzle 3 by gas phase inlet 2 under 55 ℃, the gas speed that sprays from gas nozzle 3 is 178m/s, SO
3/ alkylbenzene raw materials components mole ratio 1.05: 1, SO
3/ air gas mixture is with organic materials contact and spray in the reactor kettle 7 from atomizing mouth 5 and react, and the reaction time in the reactor kettle is 2 seconds, sulfonating reaction product that obtains and unreacted SO
3After/air gas mixture is discharged from product outlet 8, carry out gas-liquid separation, liquid phase is after cooling, continue reaction 40min down at 50 ℃～55 ℃, under agitation add 1.8kg/h water then, at 50 ℃～55 ℃ following hydrolysis 15min, be neutralized to pH8 with sodium hydrate aqueous solution and promptly obtain the finished product sodium alkyl benzene sulfonate.
Embodiment 2: the sulfonation of toluene
Toluene (average molar mass: 92) under 5 ℃～10 ℃ with the flow velocity of 5.8kg/h continuously by SO
3The liquid phase inlet 1 of gas blowing type sulfonation reactor enters liquid distribution chamber 4, enters atomizing mouth 5 through atomizing mouth 5 top overflows again, flows downward SO along atomizing mouth 5 inwalls then
3/ air (volume ratio 6%) mist under 55 ℃ by SO
3The gas phase inlet 2 of gas blowing type sulfonation reactor enters gas nozzle 3, and the gas speed that sprays from gas nozzle 3 is 218m/s, SO
3/ alkylbenzene raw materials components mole ratio 1.03: 1, SO
3/ air gas mixture is with organic materials contact and go in the reactor kettle 7 from atomizing mouth spray 5 and react, and the reaction time in reactor kettle 7 is 1 second, sulfonating reaction product that obtains and unreacted SO
3/ air gas mixture is from SO
3After the product outlet 8 of gas blowing type sulfonation reactor is discharged, carry out gas-liquid separation, liquid phase is after cooling, continue reaction 20min down at 15～20 ℃, under agitation add 0.6kg/h water then,, be neutralized to pH9 with potassium hydroxide aqueous solution and promptly obtain finished product at 15～20 ℃ of following hydrolysis 15min.
Embodiment 3: the sulphation of ethoxylated dodecyl alcohol (n=3)
(n=3 is hereinafter to be referred as AEO for ethoxylated dodecyl alcohol
3, average molar mass 326) under 32 ℃ with the flow velocity of 16.3kg/h continuously by SO
3The liquid phase inlet 1 of gas blowing type sulfonation reactor enters liquid distribution chamber 4, enters atomizing mouth 5 through atomizing mouth 5 top overflows again, flows downward SO along atomizing mouth 5 inwalls then
3/ air (volume ratio 3.5%) mist under 55 ℃ by SO
3The gas phase inlet 2 of gas blowing type sulfonation reactor enters gas nozzle 3 from the fast 195m/s of being of the gas of gas nozzle 3 ejections, SO
3/ alkylbenzene raw materials components mole ratio 1.03: 1, SO
3/ air gas mixture sprays in the reactor kettle 7 with the organic materials contact and from atomizing mouth 5 reacts, and the reaction time in reactor kettle 7 is 3 seconds, sulfonating reaction product that obtains and unreacted SO
3/ air gas mixture is from SO
3After the product outlet 8 of gas blowing type sulfonation reactor is discharged, carry out gas-liquid separation, liquid phase continues reaction 10min down at 45 ℃ after cooling, use NH
4The OH aqueous solution is neutralized to pH 6.5, obtains finished product AES (ethoxylated dodecyl alcohol ammonium sulfate).
Embodiment 4: the sulfonation of alkyl diphenyl ether
C
14～16Alkyl diphenyl ether (average molar mass 456) under 95 ℃ with the flow velocity of 22.8kg/h continuously by SO
3The liquid phase inlet 1 of gas blowing type sulfonation reactor enters liquid distribution chamber 4, enters atomizing mouth 5 through atomizing mouth 5 top overflows again, flows downward SO along atomizing mouth 5 inwalls then
3/ air (volume ratio 13%) mist under 55 ℃ by SO
3The gas phase inlet 2 of gas blowing type sulfonation reactor enters gas nozzle 3 from the fast 128m/s of being of the gas of gas nozzle 3 ejections, SO
3/ alkylbenzene raw materials components mole ratio 2.0: 1, SO
3/ air gas mixture sprays in the reactor kettle 7 with the organic materials contact and from atomizing mouth 5 reacts, and the reaction time in reactor kettle 7 is 5 seconds, sulfonating reaction product that obtains and unreacted SO
3/ air gas mixture is from SO
3After the product outlet 8 of gas blowing type sulfonation reactor is discharged, carry out gas-liquid separation, liquid phase continues reaction 80min down at 85～90 ℃ after cooling, under agitation add 2.8kg/h water then, and 85～90 ℃ of hydrolysis 30min are with Mg (OH)
2The aqueous solution is neutralized to pH7, obtains the finished product alkyl diphenyl ether sulfonic acid magnesium aqueous solution.
Embodiment 5: the sulphation of NPE (n=4)
NPE (n=4, average molar mass 384) under 45 ℃ with the flow velocity of 24.0kg/h continuously by SO
3The liquid phase inlet 1 of gas blowing type sulfonation reactor enters liquid distribution chamber 4, enters atomizing mouth 5 through atomizing mouth 5 top overflows again, flows downward SO along atomizing mouth 5 inwalls then
3/ air (volume ratio 4%) mist under 65 ℃ by SO
3The gas phase inlet 2 of gas blowing type sulfonation reactor enters gas nozzle 3 from the fast 205m/s of being of the gas of gas nozzle 3 ejections, SO
3/ alkylbenzene raw materials components mole ratio 1.04: 1, SO
3/ air gas mixture sprays in the reactor kettle 7 with the organic materials contact and from atomizing mouth 5 reacts, and the reaction time in reactor kettle 7 is 3 seconds, sulfonating reaction product that obtains and unreacted SO
3/ air gas mixture is from SO
3After the product outlet 8 of gas blowing type sulfonation reactor is discharged, carry out gas-liquid separation, liquid phase continues reaction 10min down at 45 ℃ after cooling, be neutralized to pH 6 with the triethanolamine aqueous solution, obtains finished product AES (NPE sulfuric acid triethanolamine).
Embodiment 6: the sulfonation of dibutyl naphthalene
Dibutyl naphthalene (average molar mass: 184) under 15 ℃ with the flow velocity of 11.5kg/h continuously by SO
3The liquid phase inlet 1 of gas blowing type sulfonation reactor enters liquid distribution chamber 4, enters atomizing mouth 5 through atomizing mouth 5 top overflows again, flows downward SO along atomizing mouth 5 inwalls then
3/ air (volume ratio 15%) mist under 55 ℃ by SO
3The gas phase inlet 2 of gas blowing type sulfonation reactor enters gas nozzle 3, and the gas speed that sprays from gas nozzle 3 is 173m/s, SO
3/ alkylbenzene raw materials components mole ratio 1.06: 1, SO
3/ air gas mixture is with organic materials contact and go in the reactor kettle 7 from atomizing mouth spray 5 and react, and the reaction time in reactor kettle 7 is 2 seconds, sulfonating reaction product that obtains and unreacted SO
3/ air gas mixture is from SO
3After the product outlet 8 of gas blowing type sulfonation reactor is discharged, carry out gas-liquid separation, liquid phase is after cooling, continue reaction 10min down at 15～20 ℃, under agitation add 0.3kg/h water then,, be neutralized to pH9 with aqua calcis and promptly obtain finished product at 25 ℃ of following hydrolysis 10min.
Claims (10)
1, a kind of technique for applying of SO 3 gas jetting formula sulfonation reactor is characterized in that comprising the steps:
By the aerial concentration of volume percent of sulfur trioxide is 3～15%, with SO
3/ air is mixed into mist also after filtering, and mist enters SO
3The gas nozzle of gas blowing type sulfonation reactor (3), SO during air inlet body nozzle (3)
3/ air gas mixture temperature is between 55～70 ℃, and in 50m/s～300m/s scope, organic matter enters SO from the gas speed of gas nozzle (3) ejection
3Temperature during the gas blowing type sulfonation reactor is controlled between 5 ℃～100 ℃, organic matter and SO
3Mol ratio be controlled at 1.0～2.0: between 1, organic matter and SO
3/ air gas mixture is at SO
3React in the gas blowing type sulfonation reactor, the reaction time in the reactor kettle is 1～5 second, sulfonating reaction product and unreacted SO
3/ air gas mixture is from SO
3After the product outlet (8) of gas blowing type sulfonation reactor is discharged, carry out gas-liquid separation, liquid phase is after cooling, continue reaction 10～90min down at 10～80 ℃, the water that under agitation adds sulfonic acid weight O～1.5% then, 10～80 ℃ of following hydrolysis 0～90 minute, be neutralized to pH6～9 with aqueous slkali and promptly obtain finished product;
Described SO 3 gas jetting formula sulfonation reactor, be by nozzle, reactor kettle (7) is formed, nozzle comprises gas nozzle (3), liquid distribution chamber (4), atomizing mouth (5), liquid phase feed inlet (1) and mist inlet (2), gas nozzle (3) communicates with mist inlet (2) and is fixed in top, liquid distribution chamber (4), liquid phase feed inlet (1) is positioned at the bottom of side, liquid distribution chamber (4), atomizing mouth (5) is fixed in the liquid distribution chamber (4), gas nozzle (3) bottom enters in the atomizing mouth (5), atomizing mouth (5) top is an opening, the position of atomizing mouth (5) top in liquid distribution chamber (4) is higher than liquid phase feed inlet (1) position in liquid distribution chamber (4), nozzle is fixed in reactor kettle (7) top, atomizing mouth (5) bottom enters in the reactor kettle (7), and there is product outlet (8) reactor kettle (7) lower end.
2, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 1 is characterized in that being fixed with in the described reactor kettle (7) guide shell (6), and atomizing mouth (5) bottom enters in the guide shell (6).
3,, it is characterized in that described nozzle evenly distributes with 2～60 on reactor kettle (7) top as the technique for applying of claim 1 SO 3 gas jetting formula sulfonation reactor.
4, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 1 is characterized in that described SO
3Be by combustion sulphur method, oleum acid gas formulation or liquid SO
3The evaporation preparation.
5, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 1 is characterized in that described organic matter is the alkane chain at 8～20 fatty alcohol, AEO or APES.
6, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 1 is characterized in that described unreacted SO
3/ air gas mixture recycles.
7, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 1 is characterized in that the aerial concentration of volume percent of described sulfur trioxide is 6～12%.
8, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 1 is characterized in that described alkali is inorganic base or organic base.
9, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 8 is characterized in that described inorganic base is NaOH, potassium hydroxide, ammonium hydroxide, magnesium hydroxide or calcium hydroxide.
10, the technique for applying of a kind of SO 3 gas jetting formula sulfonation reactor as claimed in claim 8 is characterized in that described organic base is MEA, diethanol amine, triethanolamine or tetraalkylammonium hydroxide.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101692063B (en) * | 2009-10-15 | 2013-02-27 | 武汉青江化工股份有限公司 | Method for detecting process and end point of sulfur trioxide sulfonation |
| CN103861544B (en) * | 2012-12-17 | 2016-07-27 | 中国石油化工股份有限公司 | A kind of impact flow reactor and application thereof |
| CN103432978B (en) * | 2013-06-22 | 2015-02-04 | 安阳市双环助剂有限责任公司 | Sulfonation reactor and use method thereof |
| CN103706288B (en) * | 2013-12-25 | 2016-08-31 | 浙江赞宇科技股份有限公司 | The fatty alcohol polyoxyethylene ether sulfate of a kind of high-load and production technology thereof |
| CN104174352A (en) * | 2014-09-04 | 2014-12-03 | 吉林化工学院 | Internal loop airlift reactor for refined white oil experiment |
| CN104785159B (en) * | 2015-03-23 | 2017-10-13 | 中国日用化学工业研究院 | A kind of technique for preparing sulfonate and sulfuric acid composite anion surfactant |
| CN105384662A (en) * | 2015-11-13 | 2016-03-09 | 无锡清杨机械制造有限公司 | Organic matter jet sulfonation reaction process |
| CN107089932B (en) * | 2017-05-26 | 2019-10-01 | 中国日用化学工业研究院 | A kind of process for sulfonation and device of alkyl diphenyl ether |
| CN111704561B (en) * | 2020-05-18 | 2023-03-03 | 中国日用化学研究院有限公司 | Method for preparing alkyl diphenyl ether sulfonate by sulfonating liquid-phase sulfur trioxide |
| CN112844295B (en) * | 2021-01-18 | 2022-12-02 | 黄河科技学院 | Multifunctional reaction device for biochemical experiments |
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Assignee: Hunan Li Chenao prestige Industrial Co., Ltd. Assignor: Chinese Daily Use Chemical Industry Research Inst. Contract record no.: 2011430000283 Denomination of invention: SO3 gas jetting sulfonation reactor and process Granted publication date: 20100127 License type: Exclusive License Open date: 20070606 Record date: 20111109 |
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Effective date of registration: 20180531 Address after: 312369 No. 19 Wei three road, Hangzhou Bay Economic and Technological Development Zone, Shangyu District, Shaoxing, Zhejiang Patentee after: Zhongguang chemical Shaoxing Co., Ltd. Address before: No. 34, Wen Yuan Lane, Taiyuan, Shanxi Province Patentee before: Chinese Daily Use Chemical Industry Research Inst. |
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