CN115245793B - Acid ester re-sulfonation device after alkyl benzene sulfonic acid sulfonation reaction and operation method - Google Patents
Acid ester re-sulfonation device after alkyl benzene sulfonic acid sulfonation reaction and operation method Download PDFInfo
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- CN115245793B CN115245793B CN202210905335.2A CN202210905335A CN115245793B CN 115245793 B CN115245793 B CN 115245793B CN 202210905335 A CN202210905335 A CN 202210905335A CN 115245793 B CN115245793 B CN 115245793B
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- 239000002253 acid Substances 0.000 title claims abstract description 115
- 150000002148 esters Chemical class 0.000 title claims abstract description 99
- 238000006277 sulfonation reaction Methods 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 24
- 150000004996 alkyl benzenes Chemical class 0.000 title claims abstract description 23
- 229940092714 benzenesulfonic acid Drugs 0.000 title abstract description 8
- 238000009826 distribution Methods 0.000 claims abstract description 44
- 239000011148 porous material Substances 0.000 claims abstract description 28
- 239000011344 liquid material Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims description 23
- 238000000926 separation method Methods 0.000 claims description 21
- 239000011552 falling film Substances 0.000 claims description 17
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 16
- 238000005192 partition Methods 0.000 claims description 7
- 239000011800 void material Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 13
- 208000012839 conversion disease Diseases 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 16
- 239000000047 product Substances 0.000 description 14
- 238000001514 detection method Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 230000019635 sulfation Effects 0.000 description 3
- 238000005670 sulfation reaction Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 230000005501 phase interface Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
- B01J10/02—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor of the thin-film type
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/247—Suited for forming thin films
-
- 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
-
- 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
- C07C303/26—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfonic acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an acid ester re-sulfonation device after an alkyl benzene sulfonic acid sulfonation reaction and an operation method thereof. The device has simple structure and reliable performance, and the discharged acid ester is prevented from staying on the conical tube wall at the bottom of the sulphonater to cause oversulphonation phenomenon due to longer stay time by redistributing the liquid material distribution pore plates; meanwhile, the acid ester re-sulphonater enables the sulphonated gas and the acid ester to carry out re-sulphonation reaction for a short time in the falling process, so that the reaction conversion rate and the raw material utilization rate are continuously improved, and the acid gas content in the tail gas removal treatment stage of the sulphonated gas is reduced.
Description
Technical Field
The invention belongs to the field of surfactant production, and relates to an acid ester re-sulfonation device after an alkyl benzene sulfonic acid (LAS) sulfonation reaction and an operation method.
Background
The sulfonation/sulfation technique mainly refers to the sulfonation/sulfation (-SO) 3 H/-OSO 3 H) The alkyl benzene sulfonic acid is one of the anionic surfactants prepared by sulfonation reaction, and is introduced into organic molecular chains through chemical reaction, plays an important role in organic synthesis, and is widely applied to the field of industrial production, such as the synthesis of anionic surfactants, dyes, drug intermediates, pesticide production and the like. The industry of alkylbenzenesulfonic acids is mainly using SO 3 The gas is used as main sulfonating agent, and sulfonic acid groups are introduced into molecular chains to enable organic matters to have surface activities such as emulsification, foaming, wetting and the like, so that the organic matters are one of important surface active agents used in washing products. The sulfonation reaction is mainly carried out by diluting SO 3 The gas and alkylbenzene are contacted in the sulfonation reactor, and after film formation in the falling film sulfonation tube, the gas and alkylbenzene downward flow along the sulfonation tube, and after contact, are reacted, and after flowing out from the falling film sulfonation tube, the gas and alkylbenzene are fed into the sulfonation reactorAnd (3) separating the acid ester from the sulfonated gas by a gas-liquid separator, and then enabling the acid ester to enter a post-treatment working section, wherein the gas is subjected to tail gas removal treatment working section.
Because the discharge hole at the bottom of the sulphonater is cone-shaped, part of acid ester can be attached to the pipe wall in the falling process, and because the sulphonation reaction is a strong exothermic reaction, the viscosity of the organic material is increased by 50-200 times in the reaction process, part of acid ester can stay on the pipe wall for a long time, the flow rate of sulphonated gas is high (the flow rate is 20-30 m/s) after the sulphonated gas comes out from the bottom of the sulphonater, and the acid ester which stays on the pipe wall is contacted with the residual SO in the acid ester after the acid ester continuously contacts with the acid gas flowing out from the sulphonation pipe of the sulphonater falling film 3 The gas continues to react to cause the phenomenon of over sulfonation, so that partial acid ester becomes dark in color, and the quality of the product is finally influenced along with the extension of the production time. In addition, in the falling process of the acid ester flowing out of the sulfonation falling film sulfonation pipe of the sulfonator, as the flow rate of the sulfonation gas is too fast and the distribution is uneven (influenced by a conical pipeline at the bottom of the sulfonator, the blocking effect on part of gas exists), the acid ester is not contacted with the sulfonation gas uniformly in the falling process of the acid ester, and the sulfonation reaction degree of part of the acid ester in the pipeline flowing process after the acid ester leaves the sulfonator is different to a certain extent, so that the acid ester is difficult to improve in the subsequent working section.
Disclosure of Invention
In order to solve the problems, the invention provides an alkyl benzene sulfonic acid sulfonation reaction post-acid ester re-sulfonation device and an operation method, wherein the acid ester after the sulfonation reaction is collected and re-distributed, so that the reaction efficiency is improved, the occurrence of side reactions is reduced, the color of a product is reduced, and the product quality is improved. The whole set of device and the operation are simple and easy to implement, and have certain practicability.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the utility model provides an acid ester re-sulfonation device after alkylbenzene sulfonic acid sulfonation reaction, includes liquid material distribution orifice plate, acid ester re-sulfonation ware and gas-liquid separator, liquid material distribution orifice plate set up in falling film sulfonation tube with between the acid ester re-sulfonation ware, liquid material distribution orifice plate is fixed in the entry of acid ester re-sulfonation ware, acid ester re-sulfonation ware is including the fixed part that is located the tip with be located a plurality of division boards of inside, the mutual parallel arrangement of division board, the export of acid ester re-sulfonation ware with gas-liquid separator is connected.
As a preferable scheme of the invention, the liquid material distribution pore plate is hexagonal, and the surface of the liquid material distribution pore plate is provided with distribution holes which are arrayed.
As a preferable scheme of the invention, the total distribution hole area on the liquid material distribution hole plate is 70-80% of the pipe diameter area of the acid ester re-sulfonator.
As a preferable scheme of the invention, the aperture of the distribution holes on the liquid material distribution pore plate is 15mm, and the hole spacing is 56mm.
As a preferable mode of the invention, the spacing of the separation plates in the acid ester re-sulphonater is 8.5mm, the width of the separation plates is 4mm, the length of the separation plates is 300mm, and the void ratio is 68%.
As a preferable scheme of the invention, the outlet of the acid ester re-sulphonating device is fixedly connected with the gas-liquid separator through a flange.
The invention also provides an operation method of the acid ester re-sulfonation device after the alkyl benzene sulfonic acid sulfonation reaction, which comprises the following steps:
1) The acid ester flows out of the falling film sulfonation pipe and enters a liquid material distribution pore plate, and flows down again through the distribution pore after being gathered on the liquid material distribution pore plate;
2) The acid ester flowing out of the liquid material distribution pore plate is left along the pipeline, enters an acid ester re-sulphonater, and after the acid ester flowing down is redistributed through the partition plates in the re-sulphonater, the acid ester and the sulphonated gas flow down after continuous contact reaction between the partition plates, and then enter a gas-liquid separator for separating the acid ester and the sulphonated gas;
3) And aging and hydrolyzing the separated acid ester to obtain the finished product alkylbenzene sulfonic acid, and treating tail gas after sulfonation reaction in an electrostatic demister and an alkaline washing tower, and detecting to be qualified and evacuating.
As a preferred embodiment of the invention, in step 2), the residence time of the acid ester in the acid ester re-sulphonater is less than or equal to 2 minutes.
The invention is based on the current production situation, and the acid ester is re-sulfonated after the sulfonation reaction of the alkylbenzene sulfonic acidThe device is used for collecting and redistributing the acid ester discharged from the sulfonation tube of the falling film of the sulfonator on the distribution pore plate, so as to avoid the acid ester contacting the tube wall or staying on the tube wall for a long time in the falling process; the redistributed acid ester flows into an acid ester re-sulphonater, and the acid ester and residual sulphonated gas continue to contact and react between the separation plates under the separation action of the separation plates, and then enter the subsequent treatment working section together. The design device of the invention is based on a gas-phase falling film sulfonation reactor, the reaction rate is controlled by gas phase, and any SO in the gas is assumed 3 Once the molecules are in contact with the organic liquid phase, the reaction conversion rate of the re-sulfonation device has the following relationship with the length L of the separation plate, the distance D between the plates and the sulfonation gas velocity v: in the assurance of SO 3 Under the condition of constant gas concentration, the larger the separation plate distance is, the more organic materials enter the space between the plates, the gas speed is reduced, and the gas phase mass transfer coefficient is basically in direct proportion to the gas speed, so that the total mass transfer equation can be known:
Øm=Kg×A×ΔC
wherein A and delta C are constants, kg is gas phase mass transfer coefficient, kg is basically proportional to gas velocity, kg is ≡v 0.8 。
This can lead to SO 3 The diffusion rate to the organic liquid phase interface is reduced, while the gas SO 3 The mass flow rate of diffusion to the organic liquid phase interface is proportional to SO 3 And the gas concentration and the volume flow of the gas are equal to m (m 3 /h), the plate length must be extended appropriately to remove residual SO 3 All reactions are absorbed, while if the plate length is maintained, the gas velocity must be doubled, which can lead to entrainment of organics into the gas phase, resulting in oversulfonation to produce undesirable black byproducts; the same applies to the reduction of the plate spacing by half, and the opposite effect to that described above can be obtained. Accordingly, by designing proper separation distance and length of separation plates of the re-sulfonation device, the re-sulfonation reaction of the acid ester can be realized, and SO (sulfur dioxide) is reduced 3 Residual quantity, reducing tail gas treatment capacity and improving product color index.
Compared with the prior art, the invention has the following beneficial effects:
1) According to the invention, after the acid ester discharged from the falling film sulfonation tube of the sulfonator is redistributed, the retention condition of the acid ester at a conical discharge hole is effectively reduced, and the phenomenon that the color is deepened and the product quality is influenced due to oversulfonation phenomenon caused by overlong retention time is avoided.
2) The device disclosed by the invention is used for enabling the acid ester discharged from the sulphonater to be in contact with the sulphonation gas in a redistribution manner in the falling process, so that the acid ester can be effectively contacted with the sulphonation gas in the falling process for performing a re-sulphonation reaction, the reaction conversion rate is improved, and meanwhile, the acid gas component in the sulphonation tail gas is reduced.
3) The device has simple structure, reliable performance and better practical applicability.
4) The invention has reliable design theory, practical feasibility, improves the color of the product, reduces the residual quantity of the acid gas in the tail gas, has certain feasibility and environmental protection in industrial production, and has better economic effect.
Drawings
Fig. 1 is a schematic diagram of the present invention.
FIG. 2 is a schematic view of a liquid distribution orifice plate of the present invention.
FIG. 3 is a schematic representation of an acid ester re-sulphonator of the present invention.
In the figure, 1. A liquid material distribution pore plate; 2. acid ester re-sulphonator; 3. a gas-liquid separator; 4. a partition plate; 5. distributing holes; 6. a falling film sulfonation tube; 7. a fixing part.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The raw materials, equipment and devices used in the invention can be purchased from the market or simply manufactured.
Referring to fig. 1, the invention firstly provides an acid ester re-sulfonation device after an alkyl benzene sulfonic acid sulfonation reaction, which comprises a liquid distribution pore plate 1, an acid ester re-sulfonation device 2 and a gas-liquid separator 3, wherein the liquid distribution pore plate 1 is arranged between a falling film sulfonation pipe 6 and the acid ester re-sulfonation device 2, the liquid distribution pore plate 1 is fixed at an inlet of the acid ester re-sulfonation device 2, the acid ester re-sulfonation device 2 comprises a fixing part 7 positioned at the end part and a plurality of separation plates 4 positioned inside, the separation plates 4 are arranged in parallel, and an outlet of the acid ester re-sulfonation device 2 is connected with the gas-liquid separator 3.
Referring to fig. 2, the liquid material distribution pore plate 1 is hexagonal, the surface of the liquid material distribution pore plate 1 is provided with distribution holes 5 distributed in an array, the total distribution hole area on the liquid material distribution pore plate 1 is 70-80% of the pipe diameter area of the acid ester re-sulphonater, the aperture of the distribution holes 5 is 15mm, and the hole spacing is 56mm.
Referring to fig. 3, the separation of the separation plates 4 in the acid ester re-sulfonator 2 was 8.5mm, the width of the separation plate 4 was 4mm, the length of the separation plate 4 was 300mm, and the void fraction was 68%.
Example 1
The method for performing the sulfonation operation of the acid ester after the sulfonation reaction of the alkylbenzene sulfonic acid provided by the embodiment comprises the following steps:
taking a gas-phase film type sulfonation production line as an example (the capacity is 3.8 tons/h of alkylbenzenesulfonic acid), the specification of a matched sulfonator is phi 800 multiplied by 8000, the outlet pipe diameter is DN450, alkylbenzene (2700 kg/h) and liquid sulfur (360 kg/h) diluent gas are subjected to falling film type contact reaction in the sulfonator, and the volume flow rate of the sulfonation gas (6300 m) 3 And/h), enabling the acid ester to flow out of a falling film sulfonation pipe at the bottom of the sulfonator, enabling the acid ester to enter the acid ester re-sulfonator after passing through a liquid material distribution pore plate, wherein the re-sulfonator consists of 16 partition plates with the thickness of 8.5mm, the plate length is 300mm, and the plate void ratio is 69%; the liquid acid ester and the sulfonated gas enter a subsequent gas-liquid separator together, the acid ester and the gas are separated and then aged and hydrolyzed to obtain a finished product LAS, and the tail gas after the sulfonation reaction enters an electrostatic demister and an alkaline washing tower for treatment, and the tail gas can be emptied after being detected to be qualified.
The sample was taken to test the final sulfonic acid data, as shown in Table 1.
TABLE 1 sulfonic acid data for finished products
| Detection item | Sulfonic acid color and luster | Active content |
| The process of the invention | 14 Klett | 97.41 |
| * Conventional production process | 25 Klett | 95.06 |
(note: conventional production process means production data obtained without installing an acid ester redistribution device).
The data of the acid gas components in the tail gas of the tail gas treatment stage of sampling and detection are shown in table 2.
TABLE 2 acid gas Components in tail gas
| Detection item | SO 2 Content of | Organic acid mist (containing SO) 3 ) Content of |
| The process of the invention | 2.01 g/m 3 | 0.032 g/m 3 |
| * Conventional production processArt | 2.03 g/m 3 | 1.13 g/m 3 |
Example 2
The method for performing the sulfonation operation of the acid ester after the sulfonation reaction of the alkylbenzene sulfonic acid provided by the embodiment comprises the following steps:
taking a gas-phase film type sulfonation production line as an example (the production capacity is 1.5 tons/h of alkylbenzenesulfonic acid), the specification of a matched sulfonator is phi 550 multiplied by 6000, the outlet pipe diameter is DN200, alkylbenzene (1130 kg/h) and liquid sulfur (150 kg/h) diluent gas are subjected to falling film type contact reaction in the sulfonator, and the volume flow rate of the sulfonation gas (2660 m) 3 And/h), enabling the acid ester to flow out of a falling film sulfonation pipe at the bottom of the sulfonator, enabling the acid ester to enter the acid ester re-sulfonator after passing through a liquid distribution pore plate, wherein the re-sulfonator consists of 16 partition plates with the thickness of 4mm, the plate length is 300mm, and the void ratio between the plates is 68%; the liquid acid ester and the sulfonated gas enter a subsequent gas-liquid separator together, the acid ester and the gas are separated and then aged and hydrolyzed to obtain a finished product LAS, and the tail gas after the sulfonation reaction enters an electrostatic demister and an alkaline washing tower for treatment, and the tail gas can be emptied after being detected to be qualified.
The sample detection finished sulfonic acid data are shown in Table 3.
TABLE 3 sulfonic acid data for finished products
| Detection item | Sulfonic acid color and luster | Active content |
| The process of the invention | 12 Klett | 97.98 |
| * Conventional production process | 22 Klett | 96.06 |
(note: conventional production process means production data obtained without installing an acid ester redistribution device).
The data of the acid gas components in the tail gas of the tail gas treatment stage of sampling and detection are shown in table 4.
TABLE 4 acid gas Components in tail gas
| Detection item | SO 2 Content of | Organic acid mist (containing SO) 3 ) Content of |
| The process of the invention | 1.96 g/m 3 | 0.039 g/m 3 |
| * Conventional production process | 2.01 g/m 3 | 1.01 g/m 3 |
As can be seen from the comparison of the data of the two examples, by installing the acid ester redistribution device, the content of active substances after the production of the alkylbenzene sulfonic acid is slightly improved, namely the sulfonation reaction conversion rate is improved,and the color and luster of the sulfonic acid are effectively improved, and the quality of the product is improved. Meanwhile, the detection data of the sulfonated tail gas show that SO in the tail gas before and after the device is applied 2 The content is not greatly different and still depends on the sulfonation air generation stage, but SO 3 The content of the organic acid mist is obviously reduced, and the front-back change of the content of the active matters is combined, so that the re-sulfonation device can promote the continuous reaction and absorption of residual acid gas and acid ester in the falling process of the plate, improve the conversion rate of sulfonation reaction, reduce the content of the acid gas in tail gas, and discharge the residual acid gas after the residual acid gas is subjected to alkali treatment and is nearly completely absorbed, and experimental data prove that the device has reliable practicability.
The invention has reliable design theory, practical feasibility, improves the color of the product, reduces the residual quantity of the acid gas in the tail gas, has certain feasibility and environmental protection in industrial production, and has better economic effect.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various modifications and additions may be made without departing from the scope of the invention. Equivalent embodiments of the present invention will be apparent to those skilled in the art having the benefit of the teachings disclosed herein, when considered in the light of the foregoing disclosure, and without departing from the spirit and scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the technical solution of the present invention.
Claims (3)
1. The acid ester re-sulfonation device after the sulfonation reaction of the alkylbenzene sulfonic acid is characterized by comprising a liquid material distribution pore plate, an acid ester re-sulfonation device and a gas-liquid separator, wherein the liquid material distribution pore plate is arranged between a falling film sulfonation tube and the acid ester re-sulfonation device, the liquid material distribution pore plate is fixed at an inlet of the acid ester re-sulfonation device, the acid ester re-sulfonation device comprises a fixing part at the end part and a plurality of separation plates inside, the separation plates are arranged in parallel, and an outlet of the acid ester re-sulfonation device is connected with the gas-liquid separator; the spacing between the separation plates in the acid ester re-sulphonation device is 8.5mm, the width of the separation plates is 4mm, the length of the separation plates is 300mm, and the void ratio is 68%; the liquid material distribution pore plate is hexagonal, and the surface of the liquid material distribution pore plate is provided with distribution holes distributed in an array manner; the total distribution hole area on the liquid material distribution hole plate is 70-80% of the pipe diameter area of the acid ester re-sulfonator; the aperture of the distribution holes on the liquid material distribution pore plate is 15mm, and the hole spacing is 56mm; and the outlet of the acid ester re-sulfonator is fixedly connected with the gas-liquid separator through a flange.
2. A method for operating the sulfonation reaction of the acid ester after the sulfonation reaction of the alkylbenzene sulfonic acid, which is characterized by adopting the sulfonation reaction of the acid ester after the sulfonation reaction of the alkylbenzene sulfonic acid according to claim 1, comprising the following steps:
1) The acid ester flows out of the falling film sulfonation pipe and enters a liquid material distribution pore plate, and flows down again through the distribution pore after being gathered on the liquid material distribution pore plate;
2) The acid ester flowing out of the liquid material distribution pore plate is left along the pipeline, enters an acid ester re-sulphonater, and after the acid ester flowing down is redistributed through the partition plates in the re-sulphonater, the acid ester and the sulphonated gas flow down after continuous contact reaction between the partition plates, and then enter a gas-liquid separator for separating the acid ester and the sulphonated gas;
3) And aging and hydrolyzing the separated acid ester to obtain the finished product alkylbenzene sulfonic acid, and treating tail gas after sulfonation reaction in an electrostatic demister and an alkaline washing tower, and detecting to be qualified and evacuating.
3. The method according to claim 2, wherein in step 2), the residence time of the acid ester in the acid ester re-sulphonator is less than or equal to 2min.
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| CN202210905335.2A CN115245793B (en) | 2022-07-29 | 2022-07-29 | Acid ester re-sulfonation device after alkyl benzene sulfonic acid sulfonation reaction and operation method |
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| CN202210905335.2A CN115245793B (en) | 2022-07-29 | 2022-07-29 | Acid ester re-sulfonation device after alkyl benzene sulfonic acid sulfonation reaction and operation method |
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| CN115245793B true CN115245793B (en) | 2024-01-16 |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1419150A (en) * | 1972-11-13 | 1975-12-24 | Lion Fat Oil Co Ltd | Continuous sulphonation process |
| EP0193677A2 (en) * | 1984-12-14 | 1986-09-10 | Imperial Chemical Industries Plc | Treatment of gas mixtures |
| JP2001002633A (en) * | 1999-06-17 | 2001-01-09 | Lion Corp | PRODUCTION OF alpha-SULFOFATTY ACID ALKYL ESTER SALT AND SULFONATION APPARATUS THEREFOR |
| CN1903839A (en) * | 2006-08-18 | 2007-01-31 | 浙江赞成科技有限公司 | Continuous preparation method of petroleum sulfonate |
| KR100843501B1 (en) * | 2007-01-29 | 2008-07-03 | 주식회사 가야에너지 | Manufacturing method of high-yield alpha-sulfo fatty acid alkyl-group ester salt using bubbling sulfonation reaction, and alpha-sulfo fatty acid alkyl-group ester salt therefrom |
| CN101423482A (en) * | 2008-11-27 | 2009-05-06 | 中国日用化学工业研究院 | Integrated method of sulphonation and neutralization reaction |
| CN112538032A (en) * | 2020-12-22 | 2021-03-23 | 赞宇科技集团股份有限公司 | Production process and production system of dodecylbenzene sulfonic acid |
| CN112694422A (en) * | 2021-01-14 | 2021-04-23 | 中国日用化学研究院有限公司 | Green continuous preparation method and device for joint production of dinonyl naphthalene disulfonic acid and alkyl benzene sulfonic acid |
| CN216936047U (en) * | 2021-08-27 | 2022-07-12 | 天津天智精细化工有限公司 | Sulfonation reactor for preparing liquid detergent sulfonic acid |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100509769C (en) * | 2006-04-27 | 2009-07-08 | 李宏才 | Preparation method of alpha-sulfo fatty acid ester salt |
-
2022
- 2022-07-29 CN CN202210905335.2A patent/CN115245793B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1419150A (en) * | 1972-11-13 | 1975-12-24 | Lion Fat Oil Co Ltd | Continuous sulphonation process |
| EP0193677A2 (en) * | 1984-12-14 | 1986-09-10 | Imperial Chemical Industries Plc | Treatment of gas mixtures |
| JP2001002633A (en) * | 1999-06-17 | 2001-01-09 | Lion Corp | PRODUCTION OF alpha-SULFOFATTY ACID ALKYL ESTER SALT AND SULFONATION APPARATUS THEREFOR |
| CN1903839A (en) * | 2006-08-18 | 2007-01-31 | 浙江赞成科技有限公司 | Continuous preparation method of petroleum sulfonate |
| KR100843501B1 (en) * | 2007-01-29 | 2008-07-03 | 주식회사 가야에너지 | Manufacturing method of high-yield alpha-sulfo fatty acid alkyl-group ester salt using bubbling sulfonation reaction, and alpha-sulfo fatty acid alkyl-group ester salt therefrom |
| CN101423482A (en) * | 2008-11-27 | 2009-05-06 | 中国日用化学工业研究院 | Integrated method of sulphonation and neutralization reaction |
| CN112538032A (en) * | 2020-12-22 | 2021-03-23 | 赞宇科技集团股份有限公司 | Production process and production system of dodecylbenzene sulfonic acid |
| CN112694422A (en) * | 2021-01-14 | 2021-04-23 | 中国日用化学研究院有限公司 | Green continuous preparation method and device for joint production of dinonyl naphthalene disulfonic acid and alkyl benzene sulfonic acid |
| CN216936047U (en) * | 2021-08-27 | 2022-07-12 | 天津天智精细化工有限公司 | Sulfonation reactor for preparing liquid detergent sulfonic acid |
Non-Patent Citations (1)
| Title |
|---|
| 烷基苯磺酸的生产工艺和老化机理研究;刘炜康 等;《广州化工》;第49卷(第12期);全文 * |
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