CN111410619A - Production method for converting sodium sulfonate into sulfonic acid - Google Patents
Production method for converting sodium sulfonate into sulfonic acid Download PDFInfo
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- CN111410619A CN111410619A CN202010174517.8A CN202010174517A CN111410619A CN 111410619 A CN111410619 A CN 111410619A CN 202010174517 A CN202010174517 A CN 202010174517A CN 111410619 A CN111410619 A CN 111410619A
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- sulfonic acid
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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
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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
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/02—Column or bed processes
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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
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
- B01J49/53—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for cationic exchangers
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Abstract
The invention discloses a production method for converting sodium sulfonate into sulfonic acid, which is characterized in that a sulfonic acid solution is obtained by passing a sodium sulfonate solution through a continuous fluid separation system filled with strong acid type cation exchange resin. By adopting the technical scheme, the invention has the beneficial effects that: the method replaces the steps of hydrochloric acid synthesis, suction filtration and the like in the traditional production method, reduces the production cost, simplifies the production method, shortens the production period, increases the total yield, and improves the efficiency and the benefit in the sulfonic acid production.
Description
Technical Field
The invention relates to the technical field of product fluid separation, in particular to a production method for converting sodium sulfonate into sulfonic acid.
Background
The general formula of the sulfonic acid is R-SO3H, R represents hydrocarbyl, strong acid and relatively large water solubility, and is used for preparing dyes, medicines and detergents, and the general formula of the sulfonic acid is R-SO3H, wherein R is hydrocarbyl, most of the sulfonic acids are synthetic products, only a few kinds of sulfonic acids such as β -aminoethanesulfonic acid NH2CH2CH2SO3H exist in nature, the sulfonic acid group is a strong water-soluble strong acid group, the sulfonic acids are water-soluble strong acid compounds, the sulfonic acid group in an aromatic sulfonic acid molecule can be replaced by hydroxyl and cyano, and is an intermediate for preparing phenol and nitrile, the sulfonic acid can be prepared by sulfonation reaction of aromatic hydrocarbon or oxidation reaction of mercaptan, chlorinated sulfone can be prepared from the sulfonic acid, the sulfonic acid has large application in organic synthesis, and the H part in the sulfonic acid molecule can be replaced by halogen atoms, amino and the like.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a production method for converting sodium sulfonate into sulfonic acid, which achieves the purposes of reducing production cost, simplifying production method, shortening production period and improving total yield.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a process for converting sodium sulfonate to sulfonic acid comprises passing a solution of sodium sulfonate through a continuous fluid separation system packed with a strongly acidic cation exchange resin to obtain a sulfonic acid solution.
Furthermore, the continuous fluid separation system is internally provided with 20 separation units, each separation unit is respectively filled with strong acid type cation exchange resin, and the continuous fluid separation system is divided into:
a product conversion zone: contains 7 separating units, and 7 separating units are divided into 2 separating units of the front section and 5 separating units of the rear section, and a forward series feeding mode is adopted. The initial feed liquid passes through 2 separation units at the front section in sequence, the discharged feed liquid enters the thin material tank and is mixed with the washing liquid at the previous section, the reverse series feeding mode is adopted, the mixed liquid in the thin material tank passes through 5 separation units at the rear section in sequence, and the outlet effluent enters the product tank.
A conversion water washing area: the resin washing machine comprises 4 separation units, adopts a forward series feeding mode, utilizes pure water to wash the resin, and enables the washing liquid to enter a thin material tank.
A dilute acid regeneration zone: contains 3 separation units, adopts the forward series feeding mode, utilizes the dilute acid in the dilute acid tank as the feed liquid, and the discharge liquid that produces is discharged as the spent acid.
An acid regeneration zone: contains 2 separation units, adopts a forward series feeding mode, the feeding liquid is hydrochloric acid with the concentration of 4 percent, and the discharging liquid enters a dilute acid tank.
A regenerated water washing area: comprises 3 separation units, adopts a forward series feeding mode, utilizes pure water to rinse the resin, and the rinse solution enters a dilute acid tank.
A material top water area: contains 1 separation unit, adopts reverse feeding mode, and the feed liquid is the feed liquid in the product jar, and the water that will remain in the separation unit is washed out with the product direct top, and the water that is pushed up recycles in continuous fluid separation system.
Wherein the product conversion zone, the conversion water washing zone, the dilute acid regeneration zone, the regeneration water washing zone and the material top water zone are sequentially arranged along the circumferential direction.
Wherein the feed rates of the product conversion zone and the top water zone are both 12-16m L/min.
Wherein the feeding speed of the conversion water washing area is 20-26m L/min.
Wherein the feeding speed of the dilute acid regeneration zone and the feeding speed of the acid regeneration zone are both 60-70m L/min.
Wherein the feeding speed of the regeneration water washing area is 28-35m L/min.
Further, in the continuous fluid separation system, the filling amount of each separation unit is 250-400 ml.
The invention has the following beneficial effects:
(1) the sodium sulfonate is converted into sulfonic acid in one step, so that the process is simplified, the cost is reduced, the production period is shortened, the yield is improved, and the yield can be improved by 10 percent through verification.
(2) The continuous fluid separation technology has the following advantages:
1) due to continuous operation, the product components and concentration are kept stable, and the matching of a downstream working section is facilitated.
2) Because of continuous production, the transfer tank and the matching are very small, the equipment is compact, the transfer tank is easy to be installed at any position and is easy to be matched with the old production process and equipment, and the occupied area is only about 10 percent of the same scale.
3) The resin dosage can be reduced by about 40 percent relative to a fixed bed system; the dosage of the regenerant is greatly reduced, and the dosage of the washing water can be saved by 50-60% to the maximum.
4) At the same time, substances having different properties can be removed or separated, so that a complicated process can be simplified.
6) The rotating speed can be automatically adjusted along with the change of the mass and the flow of the inflow fluid according to the requirements of the production process; thus ensuring an economically optimum operation.
7) The flow direction of the fluid can be connected in a counter-flow or co-flow manner according to the convenience of the production process.
8) Due to the adoption of a plurality of separation units, the production method flow can be flexibly changed.
Drawings
FIG. 1 is a schematic view of a continuous fluid separation system of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
The invention aims to provide an improved sulfonic acid production method based on an advanced separation method of a continuous fluid separation device aiming at the defects of complicated steps, low yield, high cost, large wastewater quantity and the like of the existing sulfonic acid production method, so as to achieve the purposes of reducing the production cost, simplifying the production method, shortening the production period and improving the total yield.
The technical scheme of the invention is as follows: the advanced separation method of the continuous fluid separation device is adopted, the functions of evaporation, acid conversion, suction filtration and other steps in the traditional method are replaced, and the sodium sulfonate is converted into sulfonic acid in one step. The design improvement production method comprises the following processes:
the sodium sulfonate solution-raw material tank-continuous fluid separation device-sulfonic acid-enters into downstream working section, and the specific method of the invention is that the sodium sulfonate passes through a separation unit in the continuous fluid separation device filled with strong acid cation resin. In the unit of the continuous fluid separation device, sodium is exchanged with hydrogen ions on resin, the effluent is product sulfonic acid, the exchanged resin enters a regeneration zone along with the rotation of the system, and is subjected to regeneration activation of hydrochloric acid in the regeneration zone, so that the converted resin enters the exchange zone again to continuously produce the sulfonic acid.
The continuous fluid separation device technology used in the method realizes the steps of exchange, water washing, regeneration and the like according to the time lapse in the traditional production in a continuous production method, continuously feeds materials and continuously discharges products, and completely renovates the traditional fixed bed technology. In the invention, a plurality of intermediate links in the traditional production method are also saved. Within the continuous separation process: washing water, chemical reagents and the like are recycled in the system, and a large intermediate tank of the traditional fixed bed method, namely batch application is not needed. Simultaneously, due to the continuous operation of the continuous fluid separation device and the sequential switching of the fluid distribution valves, each separation unit can pump liquids of different media such as: raw materials, water, different chemical reagents, etc.
As shown in FIG. 1, the continuous fluid separation apparatus of the present invention, which was developed by the present company, was used, and a strong acid cation resin was used, and the design throughput was 0.9L/H, and the filling amount of each resin was 270ml according to the characteristics of sodium sulfonate itself, and the apparatus was divided into the following sections:
(1) and a product conversion zone (13-19 units), wherein sodium sulfonate feeding raw material liquid 13 and 14 are adopted, wherein outlet liquid 14 and outlet liquid 12 are mixed and then jointly enter a 15-19 series connection, the material liquid is in a forward feeding mode, the thinner is in a backward feeding mode, and the feeding speed is 15 ml/min.
(2) And a water conversion washing area (9-12 units) adopts a single-string positive feeding mode, the outlet of the water conversion washing area is merged into the inlet 15, and the water inlet speed is 24 ml/min.
(3) Regeneration zone (4-8 units), wherein 4-5 is about 4% hydrochloric acid, 5 outlet liquid and 3 outlet liquid are mixed and then enter 6-8, the feed liquid is in positive feed mode, and the feed speed is 65 ml/min.
(4) The regeneration water washing zone (1-3 units) washes the acid remaining in the resin tank and returns directly to the regeneration zone intermediate tank at a feed rate of 30 ml/min.
(5) And a material top water area (20 units) adopts a reverse feeding mode to directly top wash out the water remained in the resin column by the product, so that the concentration of the product is improved, and the part can be recycled by water at a feeding flow rate of 14 ml/min.
Analysis of results
(1) Product yield
In the production method, the continuous fluid separation device technology replaces the functions of the original acid synthesis transformation and other steps, the sodium sulfonate is converted into sulfonic acid in one step, and the removal rate of sodium ions in the step can reach more than 99.8 percent, as shown in table 1.
Table 1: sodium ion removal rate in sodium sulfonate continuous fluid separation experiment
Compared with the prior art:
the acid consumption is saved by 20%;
the product yield is improved by 10 percent;
the purity of the product is improved by 20 percent.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A process for the production of sodium sulfonate to sulfonic acid, characterized by: and (3) passing the sodium sulfonate solution through a continuous fluid separation system filled with strong acid type cation exchange resin to obtain the sulfonic acid solution.
2. A process for the production of sodium sulfonate to sulfonic acid according to claim 1 wherein: the continuous fluid separation system is internally provided with 20 separation units, each separation unit is respectively filled with strong acid type cation exchange resin, and the continuous fluid separation system comprises:
a product conversion zone: the device comprises 7 separation units, wherein the 7 separation units are divided into 2 separation units at the front section and 5 separation units at the rear section, a forward series feeding mode is adopted, initial feed liquid sequentially passes through the 2 separation units at the front section, discharged feed liquid enters a thin material tank and is mixed with water washing liquid at the previous section, a reverse series feeding mode is adopted, mixed liquid in the thin material tank sequentially passes through the 5 separation units at the rear section, and outlet effluent enters a product tank;
a conversion water washing area: the resin washing device comprises 4 separation units, wherein the resin is washed clean by pure water in a forward serial feeding mode, and the washing liquid enters a thin material tank;
a dilute acid regeneration zone: comprises 3 separation units, adopts a forward series feeding mode, utilizes dilute acid in a dilute acid tank as feeding liquid, and discharges the generated discharge liquid as waste acid;
an acid regeneration zone: the device comprises 2 separation units, a forward series feeding mode is adopted, feeding liquid is hydrochloric acid with the concentration of 4%, and discharging liquid enters a dilute acid tank;
a regenerated water washing area: the resin leaching device comprises 3 separation units, wherein the resin is leached by pure water in a forward serial feeding mode, and leaching liquid enters a dilute acid tank;
a material top water area: contains 1 separation unit, adopts reverse feeding mode, and the feed liquid is the feed liquid in the product jar, and the water that will remain in the separation unit is washed out with the product direct top, and the water that is pushed up recycles in continuous fluid separation system.
3. A process for the production of sodium sulfonate to sulfonic acid according to claim 2 wherein: the product conversion area, the conversion water washing area, the dilute acid regeneration area, the regeneration water washing area and the material top water area are sequentially arranged along the circumferential direction.
4. The process of claim 2, wherein the feed rates to the product conversion zone and the aqueous topping zone are each from 12 to 16m L/min.
5. The process for preparing sulfonic acid from sodium sulfonate as claimed in claim 1, wherein the feed rate of said water-washing conversion zone is 20-26m L/min.
6. The process of claim 1, wherein the dilute acid regeneration zone and the acid regeneration zone are both fed at a rate of 60-70m L/min.
7. The process for preparing sulfonic acid from sodium sulfonate as claimed in claim 1, wherein the feed rate of said regeneration water washing zone is 28-35m L/min.
8. A process for the production of sodium sulfonate into sulfonic acid according to any one of claims 2 to 7, wherein: in the continuous fluid separation system, the filling amount of each separation unit is 250-400 ml.
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| CN202010174517.8A CN111410619A (en) | 2020-03-13 | 2020-03-13 | Production method for converting sodium sulfonate into sulfonic acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174856A (en) * | 2020-10-26 | 2021-01-05 | 湖北吉和昌化工科技有限公司 | Purification production process of organic sulfonic acid |
| CN114229850A (en) * | 2021-12-17 | 2022-03-25 | 厦门世达膜科技有限公司 | Production method for converting sodium silicate into silicic acid |
| CN114230493A (en) * | 2021-12-24 | 2022-03-25 | 江阴华昌食品添加剂有限公司 | Automatic continuous ion exchange device system for large-scale extraction and production of taurine and preparation process of taurine |
| CN114369116A (en) * | 2021-12-22 | 2022-04-19 | 厦门世达膜科技有限公司 | Method for extracting high-purity phytic acid |
| CN114369043A (en) * | 2021-12-22 | 2022-04-19 | 厦门世达膜科技有限公司 | Process for preparing taurine by adopting continuous ion exchange method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174856A (en) * | 2020-10-26 | 2021-01-05 | 湖北吉和昌化工科技有限公司 | Purification production process of organic sulfonic acid |
| CN112174856B (en) * | 2020-10-26 | 2023-03-24 | 湖北吉和昌化工科技有限公司 | Purification production process of organic sulfonic acid |
| CN114229850A (en) * | 2021-12-17 | 2022-03-25 | 厦门世达膜科技有限公司 | Production method for converting sodium silicate into silicic acid |
| CN114369116A (en) * | 2021-12-22 | 2022-04-19 | 厦门世达膜科技有限公司 | Method for extracting high-purity phytic acid |
| CN114369043A (en) * | 2021-12-22 | 2022-04-19 | 厦门世达膜科技有限公司 | Process for preparing taurine by adopting continuous ion exchange method |
| CN114230493A (en) * | 2021-12-24 | 2022-03-25 | 江阴华昌食品添加剂有限公司 | Automatic continuous ion exchange device system for large-scale extraction and production of taurine and preparation process of taurine |
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Application publication date: 20200714 Assignee: Xiamen Shida membrane Engineering Co.,Ltd. Assignor: XIAMEN STARMEM TECHNOLOGY CO.,LTD. Contract record no.: X2021980014821 Denomination of invention: A production method for converting sodium sulfonate into sulfonic acid License type: Exclusive License Record date: 20211221 |
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Application publication date: 20200714 |