CN-224221315-U - Continuous production system for 1, 3-propane sultone

CN224221315UCN 224221315 UCN224221315 UCN 224221315UCN-224221315-U

Abstract

The utility model provides a continuous production system of 1, 3-propane sultone, which comprises a synthesis unit, a nanofiltration separation unit, a cation exchange unit, a falling film concentration unit and a molecular distillation unit which are sequentially in fluid communication, wherein the synthesis unit precisely controls reaction conditions by adopting a pipeline reactor, realizes continuous feeding and continuous reaction, the nanofiltration separation unit adopts nanofiltration equipment to realize rapid separation of products with different molecular weights and small molecular substances, improves the safety of the system, the cation exchange unit obtains 3-hydroxy propane sulfonic acid aqueous solution through a resin tower, then the 3-hydroxy propane sulfonic acid aqueous solution is evaporated and concentrated through a falling film evaporator of the falling film concentration unit, the concentrated solution is sent into a molecular distillation unit for esterification distillation, the product is heated uniformly and heated for a short time, the quality of the 1, 3-propane sultone product is improved, the byproduct production rate is reduced, and the safe and continuous production is realized.

Inventors

ZHA ZHIQIANG
DONG CHAO
QI PENGWEI
Chao Zhongjian

Assignees

江西德思化学有限公司

Dates

Publication Date: 20260512
Application Date: 20250423

Claims (10)

1. A continuous production system of 1, 3-propane sultone is characterized by comprising a synthesis unit, a nanofiltration separation unit, a cation exchange unit, a falling film concentration unit and a molecular distillation unit which are sequentially in fluid communication; The synthesis unit comprises a pipeline reactor (3) provided with a premixed material inlet and a reacted material outlet; The nanofiltration separation unit comprises nanofiltration equipment (4) which is provided with a post-reaction material inlet, a thin liquid outlet and a thick liquid outlet, wherein the post-reaction material inlet is communicated with the post-reaction material outlet of the pipeline reactor (3); the cation exchange unit comprises a resin tower (5) provided with a concentrated solution inlet and a 3-hydroxy propane sulfonic acid aqueous solution outlet, wherein the concentrated solution inlet is communicated with the concentrated solution outlet of the nanofiltration equipment (4); The falling film concentration unit comprises a falling film evaporator (6) which is provided with a 3-hydroxy propane sulfonic acid aqueous solution inlet and a concentrated solution outlet, wherein the 3-hydroxy propane sulfonic acid aqueous solution inlet is communicated with the 3-hydroxy propane sulfonic acid aqueous solution outlet of the resin tower (5); The molecular distillation unit comprises a molecular distiller (9) provided with a concentrated solution inlet and a 1, 3-propane sultone outlet, wherein the concentrated solution inlet is communicated with a concentrated solution outlet of the falling film evaporator (6).
2. The continuous production system of 1, 3-propane sultone according to claim 1, wherein the synthesis unit further comprises a first static mixer (1) and a second static mixer (2) which are sequentially communicated through pipelines, wherein the first static mixer (1) is provided with a sodium sulfite aqueous solution inlet, a sodium metabisulfite aqueous solution inlet and a mixed liquid outlet, the second static mixer (2) is provided with a mixed liquid inlet, an allyl alcohol/catalyst system inlet and a premixed material outlet, the mixed liquid inlet is communicated with the mixed liquid outlet of the first static mixer, and the premixed material outlet is communicated with the premixed material inlet of the pipeline reactor (3).
3. The continuous production system of 1, 3-propane sultone according to claim 2, wherein a pH regulator is arranged on a communicating pipeline between the first static mixer (1) and the second static mixer (2).
4. The continuous production system of 1, 3-propane sultone according to claim 1, wherein a reflux pipeline is arranged outside the nanofiltration device (4) and used for refluxing part of concentrated solution output by a concentrated solution outlet into the nanofiltration device (4), and/or a nanofiltration membrane of the nanofiltration device adopts a polyamide membrane, a sulfonated polyether sulfone membrane or a ceramic membrane with a molecular weight cut-off of more than 150, and/or a cation exchange resin is filled in the resin tower (5).
5. The continuous production system of 1, 3-propane sultone according to claim 1, characterized in that the falling film concentration unit further comprises a falling film receiving tank (7), wherein an inlet of the falling film receiving tank (7) is communicated with a concentrated solution outlet of the falling film evaporator (6), an outlet pipeline of the falling film receiving tank (7) is divided into two branches, a first branch is used for refluxing part of concentrated solution to the falling film evaporator (6), a second branch is used for conveying the rest of concentrated solution to the molecular distiller (9), and/or the falling film evaporator (6) adopts steam heat exchange.
6. The continuous production system of 1, 3-propane sultone according to claim 1, characterized in that the falling film concentration unit further comprises a gas-liquid separator (8), the inlet of the gas-liquid separator (8) is communicated with the light component outlet at the top of the falling film evaporator (6).
7. The continuous production system of 1, 3-propane sultone according to claim 1, characterized in that the molecular distillation unit further comprises a heavy slag receiving tank (10) and a product receiving tank (11), the heavy slag receiving tank (10) is communicated with a heavy component outlet at the bottom of the molecular still (9) for collecting heavy components, and the product receiving tank (11) is communicated with a1, 3-propane sultone outlet of the molecular still (9) for collecting products.
8. The continuous production system of 1, 3-propane sultone according to claim 1, characterized in that the molecular distillation unit further comprises a condenser (12) and a light fraction receiving tank (13), the inlet of the condenser being in communication with the light fraction outlet at the top of the molecular still (9), the outlet of the condenser (12) being in communication with the inlet of the light fraction receiving tank (13).
9. The continuous production system of 1, 3-propane sultone according to claim 8, characterized in that the condenser (12) is in communication with a vacuum system.
10. The continuous production system of 1, 3-propane sultone according to claim 5, wherein a delivery pump is arranged on an outlet pipeline of the falling film receiving tank (7), and the delivery pump is positioned between an outlet of the falling film receiving tank (7) and a node where two branches are positioned.

Description

Continuous production system for 1, 3-propane sultone Technical Field The utility model relates to the technical field of 1, 3-propane sultone production, in particular to a continuous production system of 1, 3-propane sultone. Background 1,3-Propane sultone (1, 3-Propane Sultone, 1,3-PS for short) is used as a high-efficiency sulfopropylation reagent, and a cyclic sulfonate group in a molecular structure of the 1,3-propane sultone has high reactivity and plays an important role in the field of organic synthesis. Industrially, 1,3-PS is widely used not only for synthesis of electroplating intermediates, dye dispersants and ink resins, but also for construction of sulfonic acid drug carriers (e.g. antiviral tenofovir prodrugs) in pharmaceutical chemistry. In recent years, with the explosive growth of new energy industry, high-purity 1,3-PS (acidity <20ppm and moisture <50 ppm) can be used as an electrolyte additive of a lithium ion battery, so that the stability of an electrode/electrolyte interface can be effectively improved, and the cycle life and storage stability of the battery can be prolonged. However, the current industrial production is still dominated by a batch method, and the inherent defects of the industrial production are serious constraints on industrial upgrading (1) the quality consistency bottleneck is that the fluctuation of the acidity of a product is up to 50-200ppm due to batch feeding error (+ -5%) and uneven mass transfer of a reactor, the requirement of battery grade purity is difficult to meet, (2) the efficiency and the safety contradiction are that the single batch reaction-purification period exceeds 12 hours, the manual operation of high-risk materials such as sulfuryl chloride (virulent, LD 50=25 mg/kg) and acrylic ester (inflammable and explosive) is involved, and (3) the environmental protection cost is increased, wherein the sulfur-containing waste water is generated per ton of the product, and the waste gas treatment energy consumption is about 18% of the production cost. In face of the severe requirements of the ever-increasing global 1,3-PS demand and the high-end application scene on the consistency of materials, the development of a full-flow continuous production system has become an urgent requirement of the industry. The Chinese patent application CN207623763U discloses an automatic control production system of 1, 3-propane sultone, which forms a control loop through each sensor, a motor, a heater, a nitrogen replacement valve, a tail gas discharge valve and a PLC (programmable logic controller) arranged on a 1, 3-propane sultone production device, realizes full-automatic and accurate control of reaction raw material supply, reaction temperature, nitrogen replacement, tail gas discharge and the like in the 1, 3-propane sultone production device, only relates to automatic control of a reaction stage, and cannot realize continuous operation of the whole production system. Therefore, the continuous 1, 3-propane sultone production system is provided, so that the production efficiency and the production safety of the 1, 3-propane sultone are improved, the personnel exposure is reduced, and the continuous clean production is realized. Disclosure of utility model Aiming at the situation, the utility model provides a continuous production system of 1, 3-propane sultone, which improves the production efficiency, the production safety and the product quality, and has low occurrence rate of side reaction. The technical scheme for solving the problems is as follows: A continuous production system of 1, 3-propane sultone comprises a synthesis unit, a nanofiltration separation unit, a cation exchange unit, a falling film concentration unit and a molecular distillation unit which are sequentially in fluid communication; The synthesis unit comprises a pipeline reactor, wherein the pipeline reactor is provided with a premix material inlet and a premix material outlet; The nanofiltration separation unit comprises nanofiltration equipment, wherein the nanofiltration equipment is provided with a material inlet, a thin liquid outlet and a thick liquid outlet, and the material inlet is communicated with the outlet of the pipeline reactor; The cation exchange unit comprises a resin tower, wherein the resin tower is provided with a concentrated solution inlet and a 3-hydroxy propane sulfonic acid aqueous solution outlet, and the concentrated solution inlet is communicated with the concentrated solution outlet of the nanofiltration equipment; The falling film concentration unit comprises a falling film evaporator, wherein the falling film evaporator is provided with a 3-hydroxy propane sulfonic acid aqueous solution inlet and a concentrated solution outlet, and the 3-hydroxy propane sulfonic acid aqueous solution inlet is communicated with the 3-hydroxy propane sulfonic acid aqueous solution outlet of the resin tower; The molecular distillation unit comprises a molecular distiller, and comp