CN107089932A - The process for sulfonation and device of a kind of alkyl diphenyl ether - Google Patents
The process for sulfonation and device of a kind of alkyl diphenyl ether Download PDFInfo
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- CN107089932A CN107089932A CN201710382935.4A CN201710382935A CN107089932A CN 107089932 A CN107089932 A CN 107089932A CN 201710382935 A CN201710382935 A CN 201710382935A CN 107089932 A CN107089932 A CN 107089932A
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- sulfonation
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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
- C07C303/04—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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Abstract
The present invention relates to a kind of process for sulfonation of alkyl diphenyl ether, specially gas SO3, alkyl diphenyl ether and atent solvent mixture first in film sulfonator in carrying out preliminary sulfonation at 10 35 DEG C, then proceed to carry out further sulfonation in 10 80 DEG C in autoclave sulphonator, solvent recovery tank is sent into after finally the atent solvent in product after further sulfonation is reclaimed through evaporative condenser, tail gas enters exhaust treatment system after being discharged through exhaust outlet, obtains alkyl diphenyl ether sulfonic acid product.The present invention has process efficiency height, cost low, the features such as product purity is high, color and luster is good.
Description
Technical field
The present invention relates to a kind of process for sulfonation of alkyl diphenyl ether and device.
Background technology
Alkyl diphenyl ether sulfonate has good water solubility, surface-active and inorganic in strong acid, highly basic, high concentration because of it
There is good dissolubility and stability in salt and bleaching agent solution, and be widely used in tertiary oil recovery, it is textile printing and dyeing, daily
The fields such as chemical industry, emulsion polymerization and soil sanitation.Such current product not yet realizes industrialized production at home, product all according to
Rely import.Patent CN 103265460 discloses a kind of preparation method of alkyl diphenyl ether sulfonate, by alkyl diphenyl ether, lazy
Property organic solvent feeding sulphonation kettle, add sulfonating agent insulation sulfonation for a period of time, the standing that adds water acid out point removes waste acid water after layering
Layer, removes inert organic solvents by oil reservoir vacuum distillation, obtains alkyl diphenyl ether sulfonic acid, then neutralized obtain light yellow finished product alkyl
Diphenyl ether sulfonate.Patent CN 1915969A by after 50% oleum and alkyl diphenyl ether sulfonation under certain condition, plus
Enter isometric distilled water, stratification neutralizes to obtain crude product with NaOH solution.Xu Hujun（Fine chemistry industry, 2005,22（1）:
19-22）Report in four-neck flask, after dodecyl diphenyl oxide and chloroform are stirred, chlorosulfonic acid reaction is added dropwise
After certain time, chloroform is boiled off, after being neutralized with 20%NaOH solution, brown product is obtained.In the document reported
The domestic sulfonating agent at present on the preparation use of the intermediate alkyl hexichol ether sulfonic acid of alkyl diphenyl ether sulfonate is predominantly dense
Sulfuric acid, oleum and chlorosulfonic acid, can not only increase the difficulty of separation sulfonate product using these sulfonating agents, can also be in sulfonation
During produce substantial amounts of acid waste water or sour gas HCl so that cause environmental pollution, corrosion of equipment and cost increase；
The reactor used simultaneously is stirring " autoclave "（Reactor and flask）Reactor, the reactor is although simple in construction, device is thrown
Money is few, but residence time of material length, back-mixing are serious, side reaction is more, and product substance content is relatively low, color and luster is poor, limits
The course of industrialization of alkyl diphenyl ether sulfonate.
The content of the invention
The purpose of the present invention be overcome the deficiencies in the prior art there is provided a kind of reaction efficiency is high, product substance content is high,
Color and luster is good, alkyl diphenyl ether process for sulfonation and device of the course of reaction without " three wastes ".
The process step of the invention is as follows：
（1）Preliminary sulfonation：It is 1 in mass ratio by organic matter and atent solvent：1-5 ratio is added to organic matter/atent solvent
Stirring forms organic mixture in storage tank, is squeezed into organic mixture in film sulfonator with measuring pump, while being passed through SO3/ empty
The gaseous mixture of gas, controls the SO of preliminary sulfonating reaction process3Volume ratio with gaseous mixture is 2-5%, gas SO3With organic mixture
Mol ratio be 0.5-1.5：1, the temperature of recirculated cooling water be in 10-35 DEG C, film sulfonator the residence time be 5-8min, instead
After should terminating, stopping is passed through SO3The gaseous mixture of/air；
（2）Further sulfonation：Product after preliminary sulfonation is added in autoclave sulphonator, while being passed through SO3The mixing of/air
Gas, controls the SO of sulfonating reaction process3Volume ratio with gaseous mixture is 3-10%, gas SO3Mol ratio with organic mixture is
1-2.5：1, the temperature of recirculated cooling water be in 10-80 DEG C, kettle the residence time be 28-63min, after reaction terminates, stop being passed through
SO3The gaseous mixture of/air, obtains alkyl diphenyl ether sulfonic acid product, wherein, atent solvent enters solvent after being reclaimed through evaporative condenser
Recycling can, tail gas enters exhaust treatment system after being excluded through exhaust outlet.
Step as described above（1）In organic matter be alkyl diphenyl ether, the alkyl in its structure can be single alkane of positive structure
The monoalkyl or double alkyl of base or double alkyl or isomery.
Step as described above（1）In atent solvent for dichloromethane, 1,2- dichloroethanes, chloroform, carbon tetrachloride,
Pentane, hexane or petroleum ether etc.；
Step as described above（1）Middle SO3Volume ratio with gaseous mixture is preferably 3-4%, gas SO3With mole of organic mixture
Than for 0.5-1：1；
Step as described above（1）The temperature of middle recirculated cooling water is preferably 20-30 DEG C.
Step as described above（2）Middle SO3Volume ratio with gaseous mixture is preferably 6-8%, gas SO3With rubbing for organic mixture
You are than being 1-2：1；
Step as described above（2）The temperature of middle recirculated cooling water is preferably 25-50 DEG C.
In order to complete the purpose of the present invention, devise and realize the object of the invention device, it include film sulfonation reactor 1,
Autoclave sulfonation reactor 2, organic matter/atent solvent storage tank 3, condenser 4 and atent solvent recycling can 5, it is characterised in that membrane type
The outlet at bottom of sulfonation reactor 1 is connected with the import of autoclave sulfonation reactor 2, and the top of film sulfonation reactor 1 has gaseous mixture to enter
Mouthful, the top of film sulfonation reactor 1 is connected with organic matter/atent solvent storage tank 3, the gas vent of autoclave sulfonation reactor 2 and
Condenser 4 is connected, the connection atent solvent of condenser 4 recycling can 5, and film sulfonation reactor 1 and autoclave sulfonation reactor 2 have respectively
Cooling water intake 6 and cooling water outlet 7.
The present invention has the following advantages that compared with prior art：
1) using gas SO3When carrying out sulfonation for sulfonating agent, consumption approaches theoretical amount, and reactivity is high, and speed is fast and complete,
The reaction time is shortened, energy consumption is reduced, production efficiency is improved.Sulfonation process does not generate water, does not produce spent acid, in the absence of point
The step of from sulfonate product, simplify production stage, saved cost；
2）Film sulfonator is coupled with autoclave sulphonator, the preliminary sulfonation of first membrane type is used to alkyl diphenyl ether, then kettle
The technique of the further sulfonation of formula, can greatly shorten the residence time of raw material in a kettle., suppress the progress of side reaction, reduction
The content of inorganic salts is to not higher than 2.0% in product, and the active matter content for lifting product is not high to 60%, Klett color and lusters are not less than
In 20.
Brief description of the drawings
Fig. 1 is the schematic device of the present invention.
As illustrated, 1 being film sulfonation reactor, 2 being autoclave sulfonation reactor, 3 being organic matter/atent solvent storage tank, 4
It is condenser, 5 is atent solvent recycling can, 6 is cooling water intake, and 7 be cooling water outlet, and 8 be products export, and 9 be row
Gas port.
Embodiment
Embodiment 1
The object of the invention device is realized, it includes film sulfonation reactor 1, autoclave sulfonation reactor 2, organic matter/atent solvent
Storage tank 3, condenser 4 and atent solvent recycling can 5, it is characterised in that the outlet at bottom of film sulfonation reactor 1 and autoclave sulfonation are anti-
Answer the import of device 2 to connect, there is a combi inlet port on the top of film sulfonation reactor 1, the top of film sulfonation reactor 1 with it is organic
Thing/atent solvent storage tank 3 is connected, and the gas vent of autoclave sulfonation reactor 2 is connected with condenser 4, the connection atent solvent of condenser 4
Exhaust outlet 9 is arranged at recycling can 5, condenser top, and film sulfonation reactor 1 and autoclave sulfonation reactor 2 have cooling water water inlet respectively
Mouth 6 and cooling water outlet 7.
By the mono- dodecyl diphenyl oxides of 500Kg and 1,2- dichloroethanes according to 1：2 ratio（Mass ratio）It is added to organic
Stirring forms organic mixture in thing/atent solvent storage tank 3, is squeezed into organic mixture in film sulfonator 1 with measuring pump, together
When be passed through SO3The gaseous mixture of/air, controls the SO of preliminary sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）For 3%,
Gas SO3Mol ratio with organic mixture is 1：1, the temperature of recirculated cooling water is 20 DEG C, residence time in film sulfonator
For 6min, after preliminary sulfonating reaction terminates, stopping is passed through SO3The gaseous mixture of/air.Product after preliminary sulfonation is all squeezed into
In autoclave sulphonator 2, while being passed through SO3The gaseous mixture of/air, controls the SO of sulfonating reaction process3Gas is dense（SO3With gaseous mixture
Volume ratio）For 8%, gas SO3Mol ratio with organic mixture is 1.5：1, the residence time is 35min, recirculated cooling water in kettle
Temperature be 80 DEG C, reaction terminate after, stopping be passed through SO3After the gaseous mixture of/air, evaporation of solvent, single dodecane is obtained
Yl diphenyl ether sulfonic acid product.After product is neutralized with 32%NaOH liquid, with liquid chromatographic detection, single dodecyl diphenyl oxide disulfonic acid
The content of sodium is 65.6%, and it is 1.7% that the content of inorganic salts is measured its value according to GB/T6366-92, and color and luster is according to GB/
It is 16 that T8447-2008, which is measured its Klett value,.Single dodecyl diphenyl oxide under the same terms is carried out with tank reactor
Sulfonation, in theory in kettle the residence time be 58min.
Embodiment 2
By the double dodecyl diphenyl oxides of 500Kg and dichloromethane according to 1：1 ratio（Mass ratio）It is added to organic matter/inertia molten
Stirring forms organic mixture in agent storage tank 3, squeezes into film sulfonator 1 organic mixture with measuring pump, is passed through simultaneously
SO3The gaseous mixture of/air, controls the SO of preliminary sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）For 2%, gas
SO3Mol ratio with organic mixture is 0.8：1, the temperature of recirculated cooling water is 25 DEG C, and the residence time is in film sulfonator
7min, after preliminary sulfonating reaction terminates, stopping is passed through SO3The gaseous mixture of/air.Product after preliminary sulfonation is all squeezed into kettle
In formula sulphonator 2, while being passed through SO3The gaseous mixture of/air, controls the SO of sulfonating reaction process3Gas is dense（SO3With the body of gaseous mixture
Product ratio）For 3%, gas SO3Mol ratio with organic mixture is 2：1, the residence time is 31min in kettle）, recirculated cooling water
Temperature is 30 DEG C, after reaction terminates, and stopping is passed through SO3After the gaseous mixture of/air, evaporation of solvent, double dodecyls are obtained
Hexichol ether sulfonic acid product.After product is neutralized with 32%NaOH liquid, with liquid chromatographic detection, double disodium 4-dodecyl-2,4 '-oxydibenzenesulfonates
Content be 70.1%, it is 1.0% that the contents of inorganic salts is measured its value according to GB/T6366-92, and color and luster is according to GB/T8447-
2008 are measured its Klett value for 11.Remaining be the same as Example 1.Double dodecanes under the same terms are carried out with tank reactor
The sulfonation of yl diphenyl ether, the residence time is 44min in kettle in theory.
Embodiment 3
By 500Kg isodecyls yl diphenyl ether and chloroform according to 1：3 ratio（Mass ratio）It is added to organic matter/atent solvent storage
Stirring forms organic mixture in tank 3, is squeezed into organic mixture in film sulfonator 1 with measuring pump, while being passed through SO3/ empty
The gaseous mixture of gas, controls the SO of preliminary sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）For 4%, gas SO3With having
The mol ratio of machine mixture is 1.5：1, the temperature of recirculated cooling water is 35 DEG C, and the residence time is 7min in film sulfonator, just
After step sulfonating reaction terminates, stopping is passed through SO3The gaseous mixture of/air.Product after preliminary sulfonation is all squeezed into autoclave sulfonation
In device 2, while being passed through SO3The gaseous mixture of/air, controls the SO of sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）
For 6%, gas SO3Mol ratio with organic mixture is 2.5：1, the residence time is 63min, the temperature of recirculated cooling water in kettle
For 50 DEG C, after reaction terminates, stopping is passed through SO3After the gaseous mixture of/air, evaporation of solvent, isodecyl yl diphenyl ether sulphur is obtained
Acid product.After product is neutralized with 32%NaOH liquid, with liquid chromatographic detection, the content of isodecyl diphenyl oxide disulfonate is
63.2%, it is 1.8% that the content of inorganic salts is measured its value according to GB/T6366-92, and color and luster is carried out according to GB/T8447-2008
Its Klett is determined for value 18.Remaining be the same as Example 1.Double dodecyl diphenyl oxides under the same terms are carried out with tank reactor
Sulfonation, in theory in kettle the residence time be 102min.
Embodiment 4
By 500Kg hexadecyl diphenyloxides and pentane according to 1：4 ratio（Mass ratio）It is added to organic matter/atent solvent storage tank
Stirring forms organic mixture in 3, is squeezed into organic mixture in film sulfonator 1 with measuring pump, while being passed through SO3/ air
Gaseous mixture, control the SO of preliminary sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）For 5%, gas SO3With it is organic
The mol ratio of mixture is 1：1, the temperature of recirculated cooling water is 10 DEG C, and the residence time is 8min, preliminary sulphur in film sulfonator
After change reaction terminates, stopping is passed through SO3The gaseous mixture of/air.Product after preliminary sulfonation is all squeezed into autoclave sulphonator 2
In, while being passed through SO3The gaseous mixture of/air, controls the SO of sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）For
7%th, gas SO3Mol ratio with organic mixture is 1.8：1, the residence time is 36min in kettle, and the temperature of recirculated cooling water is
25 DEG C, after reaction terminates, stopping is passed through SO3After the gaseous mixture of/air, evaporation of solvent, hexadecyl diphenyloxide sulphur is obtained
Acid product.After product is neutralized with 32%NaOH liquid, with liquid chromatographic detection, the content of cetyl diphenyl ether sodium disulfonate is
73.2%, it is 0.8% that the content of inorganic salts is measured its value according to GB/T6366-92, and color and luster is carried out according to GB/T8447-2008
It is 10 to determine its Klett value.Remaining be the same as Example 1.Double dodecyl diphenyl oxides under the same terms are carried out with tank reactor
Sulfonation, in theory in kettle the residence time be 56min.
Embodiment 5
By 500Kg octyl groups diphenyl ether and petroleum ether according to 1：5 ratio（Mass ratio）It is added to organic matter/atent solvent storage tank 3
Middle stirring forms organic mixture, is squeezed into organic mixture in film sulfonator 1 with measuring pump, while being passed through SO3/ air
Gaseous mixture, controls the SO of preliminary sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）For 4%, gas SO3Mixed with organic
The mol ratio of compound is 0.5：1, the temperature of recirculated cooling water is 10 DEG C, and the residence time is 5min, preliminary sulphur in film sulfonator
After change reaction terminates, stopping is passed through SO3The gaseous mixture of/air.Product after preliminary sulfonation is all squeezed into autoclave sulphonator 2
In, while being passed through SO3The gaseous mixture of/air, controls the SO of sulfonating reaction process3Gas is dense（SO3With the volume ratio of gaseous mixture）For
10%th, gas SO3Mol ratio with organic mixture is 1：1, the residence time is 28min in kettle, and the temperature of recirculated cooling water is 10
DEG C, after reaction terminates, stopping is passed through SO3After the gaseous mixture of/air, evaporation of solvent, octyl group hexichol ether sulfonic acid product is obtained.
After product is neutralized with 32%NaOH liquid, with liquid chromatographic detection, the content of octyl group diphenyl ether sodium monosulfate is 70.5%, inorganic salts
It is 1.1% that content is measured its value according to GB/T6366-92, and color and luster is measured its Klett value according to GB/T8447-2008
For 13.Remaining be the same as Example 1.The sulfonation of double dodecyl diphenyl oxides under the same terms is carried out with tank reactor, in theory
The residence time is 42min in kettle.
Claims (10)
1. a kind of process for sulfonation of alkyl diphenyl ether, it is characterised in that comprise the following steps：
（1）Preliminary sulfonation：It is 1 in mass ratio by organic matter and atent solvent：1-5 ratio is added to organic matter/atent solvent
Stirring forms organic mixture in storage tank, is squeezed into organic mixture in film sulfonator with measuring pump, while being passed through SO3/ empty
The gaseous mixture of gas, controls the SO of preliminary sulfonating reaction process3Volume ratio with gaseous mixture is 2-5%, gas SO3With organic mixture
Mol ratio be 0.5-1.5：1, the temperature of recirculated cooling water be in 10-35 DEG C, film sulfonator the residence time be 5-8min, instead
After should terminating, stopping is passed through SO3The gaseous mixture of/air；
（2）Further sulfonation：Product after preliminary sulfonation is added in autoclave sulphonator, while being passed through SO3The gaseous mixture of/air,
Control the SO of sulfonating reaction process3Volume ratio with gaseous mixture is 3-10%, gas SO3Mol ratio with organic mixture is 1-
2.5：1, the temperature of recirculated cooling water be in 10-80 DEG C, kettle the residence time be 28-63min, after reaction terminates, stop being passed through
SO3The gaseous mixture of/air, obtains alkyl diphenyl ether sulfonic acid product, wherein, atent solvent enters solvent after being reclaimed through evaporative condenser
Recycling can, tail gas enters exhaust treatment system after being excluded through exhaust outlet.
2. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（1）In it is organic
Thing is alkyl diphenyl ether, and the alkyl in its structure is the monoalkyl or double alkyl of positive structure, or isomery monoalkyl or double alkyl.
3. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（1）In inertia
Solvent is dichloromethane, 1,2- dichloroethanes, chloroform, carbon tetrachloride, pentane, hexane or petroleum ether.
4. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（1）Middle SO3With mixing
The volume ratio for closing gas is 3-4%.
5. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（1）Middle gas SO3
Mol ratio with organic mixture is 0.5-1：1.
6. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（1）Middle circulation is cold
But the temperature of water is 20-30 DEG C.
7. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（2）Middle SO3With mixing
The volume ratio for closing gas is 6-8%.
8. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（2）Middle gas SO3
Mol ratio with organic mixture is 1-2：1.
9. a kind of process for sulfonation of alkyl diphenyl ether as claimed in claim 1, it is characterised in that the step（2）Middle circulation is cold
But the temperature of water is 25-50 DEG C.
10. a kind of xanthator of alkyl diphenyl ether, it is characterised in that it includes film sulfonation reactor（1）, autoclave sulfonation it is anti-
Answer device（2）, organic matter/atent solvent storage tank（3）, condenser（4）With atent solvent recycling can（5）, it is characterised in that membrane type sulphur
Change reactor（1）Outlet at bottom and autoclave sulfonation reactor（2）Import connection, film sulfonation reactor（1）There is mixing on top
Gas import, film sulfonation reactor（1）Top and organic matter/atent solvent storage tank（3）Connection, autoclave sulfonation reactor（2）
Gas vent and condenser（4）Connection, condenser（4）Connect atent solvent recycling can（5）, film sulfonation reactor（1）And kettle
Formula sulfonation reactor（2）There is cooling water intake respectively（6）And cooling water outlet（7）.
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| CN109293534A (en) * | 2018-09-19 | 2019-02-01 | 中国日用化学研究院有限公司 | A kind of preparation method and device of alkyl diphenyl ether sulfonate |
| CN109351316A (en) * | 2018-12-22 | 2019-02-19 | 山东大明精细化工有限公司 | It is a kind of for producing the tank reactor and its application method of surfactant |
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| CN115745850B (en) * | 2022-11-23 | 2024-06-04 | 深圳智微通科技有限公司 | Method for continuous flow production of sodium dodecyl diphenyl ether sulfonate |
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| CN109293534B (en) * | 2018-09-19 | 2021-10-12 | 中国日用化学研究院有限公司 | Preparation method and device of alkyl diphenyl ether sulfonate |
| CN109351316A (en) * | 2018-12-22 | 2019-02-19 | 山东大明精细化工有限公司 | It is a kind of for producing the tank reactor and its application method of surfactant |
| CN111704561A (en) * | 2020-05-18 | 2020-09-25 | 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 |
| 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 |
| CN113861082A (en) * | 2021-11-12 | 2021-12-31 | 上海昶法新材料有限公司 | Method for synthesizing alkyl diphenyl ether disulfonic acid sodium by micro-channel reactor |
| CN115745850A (en) * | 2022-11-23 | 2023-03-07 | 深圳智微通科技有限公司 | Method for continuous flow production of sodium dodecyl diphenyl ether sulfonate |
| CN115745850B (en) * | 2022-11-23 | 2024-06-04 | 深圳智微通科技有限公司 | Method for continuous flow production of sodium dodecyl diphenyl ether sulfonate |
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