CN107151194A - The technique and device of a kind of quick sulfonation neutralization reaction - Google Patents
The technique and device of a kind of quick sulfonation neutralization reaction Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B45/00—Formation or introduction of functional groups containing sulfur
- C07B45/02—Formation or introduction of functional groups containing sulfur of sulfo or sulfonyldioxy groups
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0086—Processes carried out with a view to control or to change the pH-value; Applications of buffer salts; Neutralisation reactions
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- 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
- C07C303/04—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 by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—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 by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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- 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
- C07C303/24—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfuric acids
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
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Abstract
A kind of technique of quick sulfonation neutralization reaction is to add organic matter in hypergravity sulfonation reactor, then by gas SO3Mixed with dew point less than 50 DEG C of dry airs, and be cooled to 40 50 DEG C of formation gaseous mixtures, by SO3Gas liquid ratio with Organic Ingredients is 1 1.5：1, gaseous mixture is passed through in hypergravity sulfonation reactor, sulfonating reaction is carried out at 5 130 DEG C, obtained sulfonated products are directly entered turbulent averager, and process water and buck enter turbulent averager, in 0.2 0.6MPa, the pH that mixture is neutralized at 5 80 DEG C is 8 11, gained mixture enters gas-liquid separator and carries out gas-liquid separation, and gas is discharged from the exhaust outlet on gas-liquid separator top, bottom discharging opening discharge of the fluid product from gas-liquid separator.The present invention has reaction efficiency height, the small, energy consumption of investment is low, product substance content is high, coloury advantage.
Description
Technical field
The present invention relates to a kind of technique of the quick sulfonation neutralization reaction of high viscosity compound or low vapor pressure compounds
And equipment.
Technical background
Sulfonation technology has critically important status in chemical field, is the important step for synthesizing a variety of organic products.At present
Comparative maturity and autoclave and film sulfonator are mainly by industrialized sulfonation reactor.Patent CN 101367751A are disclosed
The technique that sulfuric acid sulfonation is carried out using reactor, first adds the refined naphthalene of melting, then be proportionally added into a certain amount of in reactor
Sulfonation certain time under 105% sulfuric acid, certain temperature, obtain the sulfonated bodies that acidity is 24-27%.Although autoclave sulphonator has all
Many advantages, but such reactor efficiency is low, back-mixing is serious, side reaction is more, and equipment volume is big, prepares expense, high energy consumption.Falling film type
Sulfonation reactor have developed rapidly in recent years, and patent CN1472344A, which is disclosed, uses SO3Gas phase membrane type sulfonation method is to natural oil
Sulfonation has been carried out, has obtained that emulsifiability is good, electrolyte resistance is good, the leather fat that smell is greatly improved.But the dress
Put cooling capacity limited, hot-spot easily occur, easily coking phenomenon occur when the sulfonation applied to the distillate of viscosity higher,
If using solvent（Or sulfonation is carried out to low-steam pressure raw material）, stronger devolatilization occurs again under the conditions of atm number and gas velocity
Phenomenon, makes solvent or low-steam pressure raw material largely volatilize, and brings the problem of vent gas treatment and raw material, solvent recovery etc. are new.Meanwhile,
Traditional handicraft is needed by gas-liquid separator, aging device, line pump and connecting line, for viscosity higher after sulfonation to neutralization
Sulfonated bodies easily block or fouling is in pipeline and equipment, cause production to terminate, and highly viscous sulfonated bodies is difficult to stir, and adopts
With traditional neutralization reactor neutralization can be caused insufficient, the neutralization time is long, eventually influence the substance content of product.
Supergravity reactor is to improve the microcosmic mixed effect of fast reaction process, enhancing interphase mass transfer, rapid shifting heat
Fine reactor.Raw material is carried out after sulfonation using hypergravity sulphonator, sulfonated bodies is quickly neutralized with alkali lye can prevent height
The sulfonated bodies of viscosity is to pipeline, the obstruction of equipment formation, so as to solve the problem of traditional handicraft.
The content of the invention
It is an object of the invention to provide a kind of reaction efficiency is high, the small, energy consumption of investment is low, product substance content is high, color and luster
Technique and device that a kind of good quick sulfonation is neutralized.
The process step of the invention is as follows：
（1）Under 5kg/h-500 kg/h flow velocity, organic matter is added in hypergravity sulfonation reactor, by SO3Volume ratio is
3-20%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs, and be cooled to 40-50 DEG C of formation gaseous mixture, by SO3With
The gas liquid ratio of Organic Ingredients is 1-1.5：1, gaseous mixture is passed through in hypergravity sulfonation reactor, sulfonation is carried out at 5-130 DEG C
Reaction, the heat that sulfonating reaction process is produced is shifted by the recirculated cooling water of supergravity reactor；
（2）The sulfonated products that step (1) is obtained are directly entered turbulent averager, process water and buck respectively from technique water inlet,
Buck import enters turbulent averager, and the pressure of system maintains 0.2-0.6MPa, the pH of mixture is neutralized at 5-80 DEG C
For 8-11, the heat that N-process is produced is shifted by the recirculated cooling water of turbulent averager, and gained mixture enters gas
Liquid/gas separator carries out gas-liquid separation, and gas is discharged from the exhaust outlet on gas-liquid separator top, and fluid product is from gas-liquid separator
Bottom discharging opening discharge.
Step as described above（1）Organic matter be：Sulfonic acid after high viscosity organic matter or sulfonation is high viscosity compound
Raw material such as heavy alkyl benzene, fraction oil of petroleum, alkyl diphenyl ether, rapeseed oil, soya-bean oil, naphthalene, phenylnaphthalene, 2- chloronaphthalenes, 2- bromonaphthalenes；It is low
Vapour pressure raw material such as hexanol, octanol, isohexyl alcohol, isooctanol, hexanol APEO, octanol APEO, isohexyl alcohol polyoxy
Vinethene and isooctanol polyethoxylate.
Step as described above（2）In turbulent averager structure " 4- turbulent flow averager " that sees in Fig. 1, turbulent flow neutralization
Device can be realized without exterior power, only under the effect of system internal pressure, make fluid impact flow in turbulent averager each
Species template original paper, increases the velocity gradient of fluid motion, forms turbulent flow, so that quick, the abundant neutralization between realizing material
Reaction.
Step as described above（2）In buck used in alkali be：Sodium hydroxide, potassium hydroxide, ammoniacal liquor, MEA, two
Monoethanolamine.
In order to realize the purpose of the present invention, the device of the present invention is devised, it includes hypergravity sulfonation reactor, raw material and stored up
Tank, turbulent averager, gas-liquid separator, it is characterised in that the material inlet of hypergravity sulfonation reactor by feedstock pump with
Raw material storage tank is connected, and the bottom end outlet of hypergravity sulfonation reactor is connected by connecting tube with the import of turbulent averager, even
There is technique water inlet in adapter, buck import, the bottom end outlet of turbulent averager and gas-liquid separation are arranged at the top of turbulent averager
Device is connected, and the outlet of gas-liquid separator bottoms is connected with discharging pump, and exhaust outlet is arranged at gas-liquid separator top, in hypergravity sulfonation
Reactor and turbulent averager have cooling water inlet and coolant outlet respectively.
The present invention has the following advantages that compared with prior art：
The present invention using gaseous sulfur trioxide as sulfonating agent, hypergravity sulfonation reactor and turbulent averager carry out sulfonation, in
The fast reaction mode of sum, technique is simple, easy to operate, almost pollution-free to environment, and investment and operating cost are low.Using overweight
Power sulfonation reactor can make interphase mass transfer speed ratio traditional reactor improve the 1-3 order of magnitude so that reaction efficiency is improved, prevented
The phenomenon such as sulfonation and organic matter devolatilization is locally crossed in reactor, can obtain that active matter content is high, coloury sulfonated product；It is right
Product after sulfonation carries out sufficient neutralization reaction in turbulent averager rapidly, it is quickly formed readily flowed neutralization
Thing, it is to avoid the blocking of pipeline and pump that sulfonated bodies is caused in course of conveying, can obtain active matter content in 30-70wt%
Product.
This method is particularly suitable for quick sulfonation, the neutralization reaction of high viscosity compound or low vapor pressure compounds.
Brief description of the drawings
Fig. 1 is the schematic device of the present invention.
As illustrated, 1 be hypergravity sulfonation reactor, 2 be feedstock pump, 3 be raw material storage tank, 4 be turbulent averager,
5 it is gas-liquid separator, 6 is discharging pump, 7 is connecting tube, and 8 be technique water inlet, and 9 be buck import, and 10 be products export, and 11 are
Cooling water inlet, 12 be coolant outlet, and 13 be exhaust outlet.
Embodiment
Embodiment 1
The device of the present invention, it includes hypergravity sulfonation reactor 1, raw material storage tank 3, turbulent averager 4, gas-liquid separator 5, its
It is characterised by that the material inlet of hypergravity sulfonation reactor 1 is connected by feedstock pump 2 with raw material storage tank 3, hypergravity sulfonation
The bottom end outlet of reactor 1 is connected by connecting tube 7 with the import of turbulent averager 4, there is technique water inlet 8 in connecting tube 7,
Buck import 9 is arranged at the top of turbulent averager 4, and the bottom end outlet of turbulent averager 4 is connected with gas-liquid separator 5, gas-liquid separation
The bottoms of device 5 outlet 10 is connected with discharging pump 6, and exhaust outlet 13 is arranged at the top of gas-liquid separator 5, in hypergravity sulfonation reactor 1
There are cooling water inlet 11 and coolant outlet 12 respectively with turbulent averager 4.
Under the flow velocity that 5kg/h is controlled by measuring pump 2, heavy alkyl benzene is pumped into from raw material storage tank 3 by raw material pump 2 overweight
In power sulfonation reactor 1, by SO3Volume ratio is 8%, by gas SO3Mix, and be cooled to less than -50 DEG C of dry airs with dew point
50 DEG C of formation gaseous mixtures, by SO3Gas liquid ratio with Organic Ingredients is 1.15：1, gaseous mixture is continuously passed through to hypergravity sulfonating reaction
In device 1, the pressure of reaction system is 0.2MPa, into the SO of hypergravity sulfonation reactor3With heavy alkyl benzene fast reaction, produce
Heat shifted by recirculated cooling water, control sulfonating reaction temperature be 50 DEG C.Product after sulfonation is directly entered disorderly
Averager 4 is flowed, process water and potassium hydroxide base water enter turbulent averager 4 from technique water inlet 8, buck import 9 respectively, realized
Instantaneous Situation is neutralized, and the pH that mixture is neutralized at 45 DEG C is 10, and the heat of N-process release is entered by recirculated cooling water
Row transfer.Active matter content is by controlling the input of process water to control 50%.Gained mixture is carried out into gas-liquid separator 5
Gas-liquid separation, gas is discharged from the exhaust outlet on the top of gas-liquid separator 5, bottom discharging opening of the fluid product from gas-liquid separator 5
Discharge.The active matter content of products obtained therefrom is measured its value for 48.1wt% according to GB/T 5173-1995, and unsulfonated oil contains
Amount is measured its value for 5.4wt% according to GB/T 11989-1989, and color and luster is measured it according to GB/T8447-2008
Klett values are 13.
Embodiment 2
Under the flow velocity that 20kg/h is controlled by measuring pump, rapeseed oil is pumped into hypergravity sulfonation from raw material storage tank 3 by raw material pump 2
In reactor 1, by SO3Volume ratio is 10%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs, and be cooled to 45 DEG C of shapes
Into gaseous mixture, by SO3Gas liquid ratio with Organic Ingredients is 1.2：1, gaseous mixture is continuously passed through in hypergravity sulfonation reactor 1,
The pressure of reaction system is 0.3MPa, into the SO of hypergravity sulfonation reactor3With rapeseed oil fast reaction, the heat of generation leads to
Cross recirculated cooling water to be shifted, the temperature for controlling sulfonating reaction is 80 DEG C.Product after sulfonation is directly entered turbulent averager
4, process water and sodium hydroxide alkali water enter turbulent averager 4 from technique water inlet 8, buck import 9 respectively, realize Instantaneous Situation
Neutralize, the pH that mixture is neutralized at 50 DEG C is 8, the heat of N-process release is shifted by recirculated cooling water.It is living
Property thing content by control process water input control 30%.Gained mixture enters gas-liquid separator 5 and carries out gas-liquid separation,
Gas is discharged from the exhaust outlet on the top of gas-liquid separator 5, bottom discharging opening discharge of the fluid product from gas-liquid separator 5.Gained
The active matter content of product is measured its value for 30.3wt% according to GB/T 5173-1995, and the content of unsulfonated oil is according to GB/
T 11989-1989 are measured its value for 1.1wt%, and it is 15 that color and luster is measured its Klett value according to GB/T8447-2008.
Embodiment 3
Under the flow velocity that 50kg/h is controlled by measuring pump, phenylnaphthalene is pumped into hypergravity sulfonation from raw material storage tank 3 by raw material pump 2
In reactor 1, by SO3Volume ratio is 20%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs, and be cooled to 50 DEG C of shapes
Into gaseous mixture, by SO3Gas liquid ratio with Organic Ingredients is 1.5：1, gaseous mixture is continuously passed through in hypergravity sulfonation reactor 1,
The pressure of reaction system is 0.6MPa, into the SO of hypergravity sulfonation reactor3With phenylnaphthalene fast reaction, the heat of generation leads to
Cross recirculated cooling water to be shifted, the temperature for controlling sulfonating reaction is 130 DEG C.Product after sulfonation is directly entered turbulent averager
4, process water and potassium hydroxide base water enter turbulent averager 4 from technique water inlet 8, buck import 9 respectively, realize Instantaneous Situation
Neutralize, the pH that mixture is neutralized at 80 DEG C is 9, the heat of N-process release is shifted by recirculated cooling water.It is living
Property thing content by control process water input control 30%.Gained mixture enters gas-liquid separator 5 and carries out gas-liquid separation,
Gas is discharged from the exhaust outlet on the top of gas-liquid separator 5, bottom discharging opening discharge of the fluid product from gas-liquid separator 5.Gained
The active matter content of product is measured its value for 31.3wt% according to GB/T 5173-1995, and the content of unsulfonated oil is according to GB/
T 11989-1989 are measured its value for 1.6wt%, and it is 14 that color and luster is measured its Klett value according to GB/T8447-2008.
Embodiment 4
Under the flow velocity that 100kg/h is controlled by measuring pump, hexanol is pumped into hypergravity sulfonation from raw material storage tank 3 by raw material pump 2
In reactor 1, by SO3Volume ratio is 4%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs, and be cooled to 40 DEG C of shapes
Into gaseous mixture, by SO3Gas liquid ratio with Organic Ingredients is 1.02：1, gaseous mixture is continuously passed through to hypergravity sulfonation reactor 1
In, the pressure of reaction system is 0.2MPa, into the SO of hypergravity sulfonation reactor3With hexanol fast reaction, the heat of generation
Shifted by recirculated cooling water, the temperature for controlling sulfonating reaction is 20 DEG C.Product after sulfonation is directly entered turbulent neutralization
Device 4, process water and ammoniacal liquor enter turbulent averager 4 from technique water inlet 8, buck import 9 respectively, realize that Instantaneous Situation is neutralized,
The pH that mixture is neutralized at 30 DEG C is 10, and the heat of N-process release is shifted by recirculated cooling water.Active matter
Content is by controlling the input of process water to control 30%.Gained mixture enters gas-liquid separator 5 and carries out gas-liquid separation, gas
Discharged from the exhaust outlet on the top of gas-liquid separator 5, bottom discharging opening discharge of the fluid product from gas-liquid separator 5.Products obtained therefrom
Active matter content be measured its value according to GB/T 5173-1995 for 30.8wt%, the content of unsulfonated oil is according to GB/T
11989-1989 is measured its value for 0.5wt%, and it is 10 that color and luster is measured its Klett value according to GB/T8447-2008.
Embodiment 5
Under the flow velocity that 200kg/h is controlled by measuring pump, octanol APEO is pumped into from raw material storage tank 3 by raw material pump 2
In hypergravity sulfonation reactor 1, by SO3Volume ratio is 5%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs, and it is cold
But to 40 DEG C of formation gaseous mixtures, by SO3Gas liquid ratio with Organic Ingredients is 1.05：1, gaseous mixture is continuously passed through to hypergravity sulphur
Change in reactor 1, the pressure of reaction system is 0.3MPa, into the SO of hypergravity sulfonation reactor3With octanol APEO
Fast reaction, the heat of generation is shifted by recirculated cooling water, and the temperature for controlling sulfonating reaction is 25 DEG C.Production after sulfonation
Product are directly entered turbulent averager 4, and process water and sodium hydroxide alkali water enter turbulent flow from technique water inlet 8, buck import 9 respectively
Averager 4, realizes that Instantaneous Situation is neutralized, and the pH that mixture is neutralized at 25 DEG C is 11, and the heat of N-process release passes through
Recirculated cooling water is shifted.Active matter content is by controlling the input of process water to control 70%.Gained mixture enters gas-liquid
Separator 5 carries out gas-liquid separation, and gas is discharged from the exhaust outlet on the top of gas-liquid separator 5, and fluid product is from gas-liquid separator 5
Bottom discharging opening discharge.The active matter content of products obtained therefrom is measured its value for 68.9wt% according to GB/T 5173-1995, not
The content of sulfonated oil is measured its value for 1.8wt% according to GB/T 11989-1989, and color and luster is measured according to GB/T3143
Its Hazen value is 9.
Embodiment 6
Under the flow velocity that 500kg/h is controlled by measuring pump, isooctanol is pumped into hypergravity sulphur from raw material storage tank 3 by raw material pump 2
Change in reactor 1, by SO3Volume ratio is 3%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs, and be cooled to 40 DEG C
Gaseous mixture is formed, by SO3Gas liquid ratio with Organic Ingredients is 1：1, gaseous mixture is continuously passed through in hypergravity sulfonation reactor 1,
The pressure of reaction system is 0.2MPa, into the SO of hypergravity sulfonation reactor3With isooctanol fast reaction, the heat of generation leads to
Cross recirculated cooling water to be shifted, the temperature for controlling sulfonating reaction is 5 DEG C.Product after sulfonation is directly entered turbulent averager 4,
Process water and aqueous monoethanolamine enter turbulent averager 4 from technique water inlet 8, buck import 9 respectively, realize Instantaneous Situation
Neutralize, the pH that mixture is neutralized at 5 DEG C is 10, the heat of N-process release is shifted by recirculated cooling water.It is living
Property thing content by control process water input control 30%.Gained mixture enters gas-liquid separator 5 and carries out gas-liquid separation,
Gas is discharged from the exhaust outlet on the top of gas-liquid separator 5, bottom discharging opening discharge of the fluid product from gas-liquid separator 5.Gained
The active matter content of product is measured its value for 30.6wt% according to GB/T 5173-1995, and the content of unsulfonated oil is according to GB/
T 11989-1989 are measured its value for 0.7wt%, and it is 8 that color and luster is measured its Klett value according to GB/T8447-2008.
Embodiment 7
Under the flow velocity that 500kg/h is controlled by measuring pump, isohexyl alcohol APEO is passed through into the pump of raw material pump 2 from raw material storage tank 3
Enter in hypergravity sulfonation reactor 1, by SO3Volume ratio is 3.5%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs,
And 40 DEG C of formation gaseous mixtures are cooled to, by SO3Gas liquid ratio with Organic Ingredients is 1.05：1, gaseous mixture is continuously passed through overweight
In power sulfonation reactor 1, the pressure of reaction system is 0.2MPa, into the SO of hypergravity sulfonation reactor3It is quick with isooctanol
Reaction, the heat of generation is shifted by recirculated cooling water, and the temperature for controlling sulfonating reaction is 25 DEG C.Product after sulfonation is straight
Tap into turbulent averager 4, process water and the diethanol amine aqueous solution enter in turbulent flow from technique water inlet 8, buck import 9 respectively
With device 4, realize that Instantaneous Situation is neutralized, the pH that mixture is neutralized at 20 DEG C is 10, the heat of N-process release is by following
Ring cooling water is shifted.Active matter content is by controlling the input of process water to control 70%.Gained mixture divides into gas-liquid
Gas-liquid separation is carried out from device 5, gas is discharged from the exhaust outlet on the top of gas-liquid separator 5, and fluid product is under gas-liquid separator 5
Portion's discharging opening discharge.The active matter content of products obtained therefrom is measured its value for 71.6wt% according to GB/T 5173-1995, non-sulphur
The content of carburetion is measured its value for 1.6wt% according to GB/T 11989-1989, and color and luster is measured it according to GB/T3143
Hazen values are 9.
Claims (4)
1. a kind of technique of quick sulfonation neutralization reaction, it is characterised in that comprise the following steps：
（1）Under 5kg/h-500 kg/h flow velocity, organic matter is added in hypergravity sulfonation reactor, by SO3Volume ratio is
3-20%, by gas SO3Mixed with dew point less than -50 DEG C of dry airs, and be cooled to 40-50 DEG C of formation gaseous mixture, by SO3With
The gas liquid ratio of Organic Ingredients is 1-1.5：1, gaseous mixture is passed through in hypergravity sulfonation reactor, sulfonation is carried out at 5-130 DEG C
Reaction, the heat that sulfonating reaction process is produced is shifted by the recirculated cooling water of supergravity reactor；
（2）The sulfonated products that step (1) is obtained are directly entered turbulent averager, process water and buck respectively from technique water inlet,
Buck import enters turbulent averager, and the pressure of system maintains 0.2-0.6MPa, the pH of mixture is neutralized at 5-80 DEG C
For 8-11, the heat that N-process is produced is shifted by the recirculated cooling water of turbulent averager, and gained mixture enters gas
Liquid/gas separator carries out gas-liquid separation, and gas is discharged from the exhaust outlet on gas-liquid separator top, and fluid product is from gas-liquid separator
Bottom discharging opening discharge.
2. a kind of technique of quick sulfonation neutralization reaction as claimed in claim 1, it is characterised in that the step（1）It is organic
Thing be heavy alkyl benzene, fraction oil of petroleum, alkyl diphenyl ether, rapeseed oil, soya-bean oil, naphthalene, phenylnaphthalene, 2- chloronaphthalenes, 2- bromonaphthalenes, hexanol,
Octanol, isohexyl alcohol, isooctanol, hexanol APEO, octanol APEO, isohexyl alcohol APEO or isooctanol polyoxy
Vinethene.
3. a kind of technique of quick sulfonation neutralization reaction as claimed in claim 1, it is characterised in that the step（2）In alkali
Alkali used in water is sodium hydroxide, potassium hydroxide, ammoniacal liquor, MEA or diethanol amine.
4. a kind of device of quick sulfonation neutralization reaction, it includes hypergravity sulfonation reactor（1）, raw material storage tank（3）, turbulent flow in
And device（4）, gas-liquid separator（5）, it is characterised in that hypergravity sulfonation reactor（1）Material inlet pass through feedstock pump
（2）With raw material storage tank（3）Connection, hypergravity sulfonation reactor（1）Bottom end outlet pass through connecting tube（7）With turbulent averager
（4）Import connection, in connecting tube（7）On have technique water inlet（8）, turbulent averager（4）Top have buck import（9）,
Turbulent averager（4）Bottom end outlet and gas-liquid separator（5）Connection, gas-liquid separator（5）Bottoms is exported（10）With going out
Expect pump（6）Connection, gas-liquid separator（5）Exhaust outlet is arranged at top（13）, in hypergravity sulfonation reactor（1）With turbulent averager
（4）There is cooling water inlet respectively（11）And coolant outlet（12）.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710382933.5A CN107151194B (en) | 2017-05-26 | 2017-05-26 | Process and device for rapid sulfonation neutralization reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710382933.5A CN107151194B (en) | 2017-05-26 | 2017-05-26 | Process and device for rapid sulfonation neutralization reaction |
Publications (2)
| Publication Number | Publication Date |
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| CN107151194A true CN107151194A (en) | 2017-09-12 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109160889A (en) * | 2018-09-18 | 2019-01-08 | 中国日用化学研究院有限公司 | A kind of technique with sulfur trioxide gas sulfonated long chain alkene and paraffins mixture |
| CN111732525A (en) * | 2020-07-31 | 2020-10-02 | 湖南丽臣奥威实业有限公司 | Method for preparing non-aqueous system fatty alcohol ether sulfuric acid organic alkanolamine salt product |
| CN111807996A (en) * | 2020-07-31 | 2020-10-23 | 湖南丽臣奥威实业有限公司 | Sulfonation method of fatty alcohol-polyoxyethylene ether |
| CN114163359A (en) * | 2021-12-14 | 2022-03-11 | 江苏亚邦染料股份有限公司 | Method for preparing 1, 4-diaminoanthraquinone-2-sulfonic acid by virtue of supergravity reactor |
| CN114570323A (en) * | 2020-11-18 | 2022-06-03 | 中国石油天然气股份有限公司 | Preparation device and preparation method of petroleum sulfonate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106606991A (en) * | 2015-10-27 | 2017-05-03 | 北京化工大学 | System device for preparing sulphonate surfactant through supergravity sulfonating method and application |
-
2017
- 2017-05-26 CN CN201710382933.5A patent/CN107151194B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106606991A (en) * | 2015-10-27 | 2017-05-03 | 北京化工大学 | System device for preparing sulphonate surfactant through supergravity sulfonating method and application |
Non-Patent Citations (2)
| Title |
|---|
| WENG ZHAN, ET AL.: "Synthesis of Petroleum Sulfonate Surfactant with Ultra-Low Interfacial Tension in Rotating Packed Bed Reactor", 《CHINA PETROLEUM PROCESSING AND PETROCHEMICAL TECHNOLOGY》 * |
| Z. WANG ET AL.: "Synthesis of heavy alkyl benzene sulfonate in a rotating packed bed combined with a stirred tank reactor", 《CHEMICAL ENGINEERING AND PROCESSING》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109160889A (en) * | 2018-09-18 | 2019-01-08 | 中国日用化学研究院有限公司 | A kind of technique with sulfur trioxide gas sulfonated long chain alkene and paraffins mixture |
| CN111732525A (en) * | 2020-07-31 | 2020-10-02 | 湖南丽臣奥威实业有限公司 | Method for preparing non-aqueous system fatty alcohol ether sulfuric acid organic alkanolamine salt product |
| CN111807996A (en) * | 2020-07-31 | 2020-10-23 | 湖南丽臣奥威实业有限公司 | Sulfonation method of fatty alcohol-polyoxyethylene ether |
| CN114570323A (en) * | 2020-11-18 | 2022-06-03 | 中国石油天然气股份有限公司 | Preparation device and preparation method of petroleum sulfonate |
| CN114570323B (en) * | 2020-11-18 | 2023-09-26 | 中国石油天然气股份有限公司 | Petroleum sulfonate preparation device and preparation method |
| CN114163359A (en) * | 2021-12-14 | 2022-03-11 | 江苏亚邦染料股份有限公司 | Method for preparing 1, 4-diaminoanthraquinone-2-sulfonic acid by virtue of supergravity reactor |
| CN114163359B (en) * | 2021-12-14 | 2023-08-08 | 江苏亚邦染料股份有限公司 | Method for preparing 1, 4-diaminoanthraquinone-2-sulfonic acid by using hypergravity reactor |
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