阅读说明：本技术 Dmss连续缩合制备工艺 (DMSS continuous condensation preparation process ) 是由 于伟华 于 2019-10-24 设计创作，主要内容包括：本发明提供一种DMSS连续缩合制备工艺,包括丁二酸二甲酯计量连续进料模块、甲醇钠计量连续进料模块、缩合模块、酸化模块、强酸计量连续进料模块、PH在线监测模块、控制系统、板框模块、滤液分层模块、第一精馏模块、回流通道、精制模块、甲醇计量连续进料模块、过滤模块、第二精馏模块、废水回收模块、干燥模块。该DMSS连续缩合制备工艺,通过PH在线监测模块实现了在线监测下的酸化连续化,取代了过去的人工取样检测和间歇酸化,提高了设备的生产能力,降低了劳动强度；同时酸化温度易控制,避免了温度高造成丁二酸二甲酯水解的情况的发生,降低了原材料消耗,丁二酸二甲酯的投入比例减小,利用率升高。(The invention provides a DMSS (dimethyl succinate) continuous condensation preparation process which comprises a dimethyl succinate metering continuous feeding module, a sodium methoxide metering continuous feeding module, a condensation module, an acidification module, a strong acid metering continuous feeding module, a PH (potential of hydrogen) online monitoring module, a control system, a plate frame module, a filtrate layering module, a first rectification module, a reflux channel, a refining module, a methanol metering continuous feeding module, a filtering module, a second rectification module, a wastewater recovery module and a drying module. According to the DMSS continuous condensation preparation process, acidification continuity under online monitoring is realized through the PH online monitoring module, the past manual sampling detection and intermittent acidification are replaced, the production capacity of equipment is improved, and the labor intensity is reduced; meanwhile, the acidification temperature is easy to control, the condition that dimethyl succinate is hydrolyzed due to high temperature is avoided, the consumption of raw materials is reduced, the input proportion of dimethyl succinate is reduced, and the utilization rate is increased.)

A DMSS continuous condensation preparation process is characterized by comprising a dimethyl succinate metering continuous feeding module, a sodium methoxide metering continuous feeding module, a condensation module, an acidification module, a strong acid metering continuous feeding module, a PH online monitoring module, a control system, a plate frame module, a filtrate layering module, a first rectification module, a backflow channel, a refining module, a methanol metering continuous feeding module, a filtering module, a second rectification module, a wastewater recovery module and a drying module, wherein the dimethyl succinate metering continuous feeding module and the sodium methoxide metering continuous feeding module are arranged in front of the condensation module according to the process flow direction, the dimethyl succinate metering continuous feeding module is communicated with the condensation module, the sodium methoxide metering continuous feeding module is communicated with the condensation module, the acidification module is arranged behind the condensation module, and the acidification module is communicated with the condensation module, the strong acid metering continuous feeding module is arranged in front of the acidification module, the strong acid metering continuous feeding module is communicated with the acidification module, the PH on-line monitoring module is connected with the acidification module, the control system is connected with the PH on-line monitoring module, the control system is connected with the strong acid metering continuous feeding module, the plate frame module is arranged behind the acidification module, the plate frame module is communicated with the acidification module, the filtrate layering module is arranged behind the plate frame module, the filtrate layering module is communicated with the plate frame module, the first rectification module is arranged behind the filtrate layering module, the first rectification module is communicated with the filtrate layering module, a backflow channel is arranged between the first rectification module and the filtrate layering module, the first rectification module is communicated with the dimethyl succinate metering continuous feeding module, the wastewater recovery module is arranged behind the filtrate layering module, and the wastewater recovery module is communicated with the filtrate layering module, the refined module sets up behind the sheet frame module, the refined module is linked together with the sheet frame module, methyl alcohol measurement serialization feed module sets up before the refined module, methyl alcohol measurement serialization feed module is linked together with the refined module, the filter module sets up behind the refined module, the filter module is linked together with the refined module, second rectification module sets up behind the filter module, second rectification module is linked together with the filter module, waste water recovery module sets up behind the second rectification module, waste water recovery module is linked together with the second rectification module, methyl alcohol measurement serialization feed module sets up behind the second rectification module, methyl alcohol measurement serialization feed module is linked together with the second rectification module, the drying module sets up behind the filter module, the drying module is linked together with the filter module, be equipped with the finished product export on the drying module, control system is the circuit board, is provided with a plurality of functional module on the circuit board.

2. The DMSS continuous condensation preparation process of claim 1, wherein the pH on-line monitoring module comprises a pH/Redox-Sensoren type pH meter.

3. The DMSS continuous condensation preparation process of claim 1 or 2, further comprising a central control system connected to the dimethyl succinate metering continuous feed module.

4. The DMSS continuous condensation preparation process according to claim 3, wherein the central control system is connected with a sodium methoxide metering continuous feeding module.

5. The DMSS continuous condensation preparation process according to claim 3, wherein the central control system is connected to a control system.

6. The DMSS continuous condensation preparation process according to claim 4, wherein the central control system is connected to a control system.

7. The DMSS continuous condensation preparation process according to claim 3, wherein the central control system is connected to a methanol metering continuous feed module.

8. The DMSS continuous condensation production process according to any one of claims 4 to 6, wherein the central control system is connected to a methanol metering continuous feed module.

Technical Field

The invention relates to the field of chemical industry, in particular to a DMSS continuous condensation preparation process.

Background

With the rapid development and development of industrialization and marketization of industries such as automobiles, real estate, advertisements and the like, society pays more and more attention to the durability of automobiles, real estate, advertisements and the like. Dimethyl succinylsuccinate is used as a high-grade pigment intermediate with high added value, is an important intermediate for preparing quinacridone high-grade organic pigments, 1, 4-cyclohexanedione and photosensitive polymers, and the competition of the domestic production market is increasingly severe at present, so that the requirements of ensuring the quality of dimethyl succinylsuccinate, enlarging the yield and reducing the production cost can be met in a fierce competition all the time.

The existing condensation process and acidification process of dimethyl succinylsuccinate usually adopt an intermittent reaction process. The intermittent reaction process is difficult to realize the accurate control of the dropping speed of sodium methoxide and the reaction temperature, the acidification temperature is high, the hydrolysis proportion of raw materials is high, the consumption of dimethyl succinate serving as a reaction raw material is high, the production cost is high, the product yield is low, the product quality is unstable, meanwhile, workers need to sample frequently during intermittent production, the labor intensity is high, the working environment is severe, the safety risk exists, and the improvement of the market competitiveness of dimethyl succinyl succinate is not facilitated.

Disclosure of Invention

The invention aims to provide a DMSS continuous condensation preparation process which reduces the production cost, improves the quality stability of a product yield agent, greatly improves the working environment of workers and reduces the labor intensity of the workers.

In order to solve the technical problems, the invention provides a DMSS (dimethyl succinate) continuous condensation preparation process, which comprises a dimethyl succinate metering continuous feeding module, a sodium methoxide metering continuous feeding module, a condensation module, an acidification module, a strong acid metering continuous feeding module, a PH on-line monitoring module, a control system, a plate frame module, a filtrate layering module, a first rectification module, a backflow channel, a refining module, a methanol metering continuous feeding module, a filtering module, a second rectification module, a wastewater recovery module and a drying module, wherein the dimethyl succinate metering continuous feeding module and the sodium methoxide metering continuous feeding module are arranged in front of the condensation module according to the process flow direction, the dimethyl succinate metering continuous feeding module is communicated with the condensation module, the sodium methoxide metering continuous feeding module is communicated with the condensation module, the acidification module is arranged behind the condensation module, the acidification module is communicated with the condensation module, the strong acid metering continuous feeding module is arranged in front of the acidification module, the strong acid metering continuous feeding module is communicated with the acidification module, the PH online monitoring module is connected with the acidification module, the control system is connected with the PH online monitoring module, the control system is connected with the strong acid metering continuous feeding module, the plate frame module is arranged behind the acidification module, the plate frame module is communicated with the acidification module, the filtrate layering module is arranged behind the plate frame module, the filtrate layering module is communicated with the plate frame module, the first rectification module is arranged behind the filtrate layering module, the first rectification module is communicated with the filtrate layering module, a backflow channel is arranged between the first rectification module and the filtrate layering module, the first rectification module is communicated with the dimethyl succinate metering continuous feeding module, the wastewater recovery module is arranged behind the filtrate layering module, the wastewater recovery module is communicated with the filtrate layering module, the refining module is arranged behind the plate frame module, the refining module is communicated with the plate frame module, the methanol metering continuous feeding module is arranged in front of the refining module, the methanol metering continuous feeding module is communicated with the refining module, the filtering module is arranged behind the refining module, the filtering module is communicated with the refining module, the second rectifying module is arranged behind the filtering module, the second rectifying module is communicated with the filtering module, the wastewater recovery module is arranged behind the second rectifying module, the wastewater recovery module is communicated with the second rectifying module, the methanol metering continuous feeding module is arranged behind the second rectifying module, the methanol metering continuous feeding module is communicated with the second rectifying module, the drying module is arranged behind the filtering module, the drying module is communicated with the filtering module, and a finished product outlet is arranged on the drying module.

Preferably, the pH on-line monitoring module comprises a pH meter of the type PH-/Redox-Sensoren.

In order to better control the reaction, the system also comprises a central control system, and the central control system is connected with the dimethyl succinate metering continuous feeding module.

For better reaction control, the central control system is connected with the sodium methoxide metering continuous feeding module.

For better control response, the central control system is connected with the control system.

For better reaction control, the central control system is connected with the methanol metering continuous feeding module.

The invention has the beneficial effects that: compared with the traditional intermittent preparation process, the DMSS continuous condensation preparation process has the advantages that the PH detection is directly carried out on the reaction liquid by adopting the PH-/Redox-Sensoren type PH meter, so that the acidification continuity under the online monitoring is realized, the manual sampling detection and the intermittent acidification in the past are replaced, the production capacity of equipment is improved, the labor intensity is reduced, and the automatic control and the continuous production are realized; meanwhile, the acidification temperature is easy to control, the condition that dimethyl succinate is hydrolyzed due to high temperature is avoided, the consumption of raw materials is reduced, the input proportion of dimethyl succinate is reduced, and the utilization rate is increased; the additional central control system can monitor, control and adjust the dimethyl succinate metering continuous feeding module, the sodium methoxide metering continuous feeding module, the methanol metering continuous feeding module and the central control system on line, so that the synthesis rate, the synthesis quality and the conversion rate of the dimethyl succinyl succinate can be controlled and improved.

Drawings

FIG. 1 is a flow chart of a continuous preparation process of dimethyl succinyl succinate of the present invention;

FIG. 2 is a structural diagram of a strong acid metering continuous feeding module of the continuous preparation process of dimethyl succinyl succinate;

FIG. 3 is a structural diagram of a refining module of the continuous preparation process of dimethyl succinyl succinate.

Description of reference numerals: 1-dimethyl succinate metering continuous feeding module; 2-sodium methoxide metering continuous feeding module; 3-a condensation module; 4-an acidification module; 5-strong acid metering continuous feeding module; 6-PH on-line monitoring module; 7-a control system; 8-a plate frame module; 9-filtrate layering module; 10-a first rectification module; 11-a return channel; 12-a refining module; 13-methanol metering continuous feeding module; 14-a filtration module; 15-a second rectification module; 16-a wastewater recovery module; 17-a drying module; 18-outlet of finished product;

Detailed Description

In order to explain technical contents, structural features, and objects and effects of the present invention in detail, the following detailed description is given with reference to the accompanying drawings in conjunction with the embodiments.

Referring to the attached figure 1, the invention provides a DMSS (dimethyl succinate) continuous condensation preparation process, which comprises a dimethyl succinate metering continuous feeding module 1, a sodium methoxide metering continuous feeding module 2, a condensation module 3, an acidification module 4, a strong acid metering continuous feeding module 5, a PH online monitoring module 6, a control system 7, a plate frame module 8, a filtrate layering module 9, a first rectification module 10, a backflow channel 11, a refining module 12, a methanol metering continuous feeding module 13, a filtering module 14, a second rectification module 15, a wastewater recovery module 16 and a drying module 17, wherein the dimethyl succinate metering continuous feeding module and the sodium methoxide metering continuous feeding module 2 are arranged in front of the condensation module 3 according to the process flow direction, the dimethyl succinate metering continuous feeding module is communicated with the condensation module 3, and the sodium methoxide metering continuous feeding module is communicated with the condensation module 3, the acidification module 4 is arranged behind the condensation module 3, the acidification module 4 is communicated with the condensation module 3, the strong acid metering continuous feeding module 5 is arranged in front of the acidification module 4, the strong acid metering continuous feeding module 5 is communicated with the acidification module 4, the PH on-line monitoring module 6 is connected with the acidification module 4, the control system 7 is connected with the PH on-line monitoring module 6, the control system 7 is connected with the strong acid metering continuous feeding module 5, the plate frame module 8 is arranged behind the acidification module 4, the plate frame module 8 is communicated with the acidification module 4, the filtrate layering module 9 is arranged behind the plate frame module 8, the filtrate layering module 9 is communicated with the plate frame module 8, the first rectification module 10 is arranged behind the filtrate layering module 9, the first rectification module 10 is communicated with the filtrate layering module 9, a backflow channel 11 is arranged between the first rectification module 10 and the filtrate layering module 9, the first rectification module 10 is communicated with the dimethyl succinate metering continuous feeding module 1, the wastewater recovery module 16 is arranged behind the filtrate layering module 9, the wastewater recovery module 16 is communicated with the filtrate layering module 9, the refining module 12 is arranged behind the plate frame module 8, the refining module 12 is communicated with the plate frame module 8, the methanol metering continuous feeding module is arranged in front of the refining module 12, the methanol metering continuous feeding module is communicated with the refining module 12, the filtering module 14 is arranged behind the refining module 12, the filtering module 14 is communicated with the refining module 12, the second rectification module 15 is arranged behind the filtering module 14, the second rectification module 15 is communicated with the filtering module 14, the wastewater recovery module 16 is arranged behind the second rectification module 15, the wastewater recovery module 16 is communicated with the second rectification module 15, the methanol metering continuous feeding module 13 is arranged behind the second rectification module 15, the methanol metering continuous feeding module 13 is communicated with the second rectification module 15, the drying module 17 is arranged behind the filtering module 14, the drying module 17 is communicated with the filtering module 14, and a finished product outlet 18 is arranged on the drying module 17.

In this embodiment, the PH on-line monitoring module 6 comprises a PH meter of the PH-/Redox-sensor type.

The DMSS continuous condensation preparation process further comprises a central control system, wherein the central control system is connected with the dimethyl succinate metering continuous feeding module 1, the central control system is connected with the sodium methoxide metering continuous feeding module 2, the central control system is connected with the control system 7, and the central control system is connected with the methanol metering continuous feeding module 13. The central control system can monitor, control and adjust the dimethyl succinate metering continuous feeding module, the sodium methoxide metering continuous feeding module 2, the methanol metering continuous feeding module 13 and the central control system on line, so that the synthesis rate, the synthesis quality and the conversion rate of the dimethyl succinyl succinate are controlled and improved.

The above central control system is a system for controlling the circuit board, and it is common knowledge of those skilled in the art that the above central control system has control circuits of these functional modules, specifically control circuits, and this is completely realizable by numerical control because how to program continuous feeding and set different feeding times and speeds.

The DMSS continuous condensation preparation process comprises the steps of firstly feeding dimethyl succinate metering continuous feeding module 1 and sodium methoxide metering continuous feeding module 2 into a condensation module 3, and then condensing into a condensation liquid through the condensation module 3; the condensation liquid enters an acidification module 4 through a condensation module 3, meanwhile, strong acid enters the acidification module 4 through a strong acid metering continuous feeding module 5, the condensation liquid is acidified in the acidification module 4 through the strong acid, the acidification degree is monitored at any time through a PH online monitoring module 6 in the acidification process, the monitoring result is fed back to a control system 7 through the PH online monitoring module 6, the control system 7 analyzes and processes the condensation liquid and controls the feeding speed of the strong acid metering continuous feeding module 5 according to the analysis result, so that the acidification continuity under online monitoring is realized, the manual sampling detection and intermittent acidification are replaced, the production capacity of equipment is improved, and the labor intensity is reduced; the condensation liquid enters a plate frame module 8 after being acidified, one part of the condensation liquid enters a filtrate layering module 9 through the plate frame module 8, the wastewater after layering is directly recycled to a golden hot wastewater recovery module 16, the other part of the condensation liquid enters a first rectification module 10, the unreacted reaction components after rectification by the first rectification module 10 flow back to a dimethyl succinate metering continuous feeding module 1, and the other reaction components flow back to the filtrate layering module 9 through a backflow channel 11; the other part of the acidified condensation liquid enters a refining module 12 through a plate frame module 8, meanwhile, methanol enters the refining module 12 through a methanol metering continuous feeding module 13, the refined condensation liquid enters a filtering module 14, the filtered filtrate enters a second rectifying module 15, the wastewater rectified by the second rectifying module 15 enters a wastewater recovery module 16, the other condensation liquid enters the methanol metering continuous feeding module 13, the filtered finished product enters a drying module 17, and the finished product can be obtained only by drying treatment.

Compared with the traditional intermittent preparation process, the DMSS continuous condensation preparation process has the advantages that the PH detection is directly carried out on the reaction liquid by adopting the PH-/Redox-Sensoren type PH meter, so that the acidification continuity under the online monitoring is realized, the manual sampling detection and the intermittent acidification in the past are replaced, the production capacity of equipment is improved, the labor intensity is reduced, and the automatic control and the continuous production are realized; meanwhile, the acidification temperature is easy to control, the condition that dimethyl succinate is hydrolyzed due to high temperature is avoided, the consumption of raw materials is reduced, the input proportion of dimethyl succinate is reduced, and the utilization rate is increased; the added central control system can monitor, control and adjust the dimethyl succinate metering continuous feeding module, the sodium methoxide metering continuous feeding module 2, the methanol metering continuous feeding module 13 and the central control system on line, thereby achieving the purpose of controlling and improving the synthesis rate, the synthesis quality and the conversion rate of the dimethyl succinyl succinate.

The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.