阅读说明：本技术 一种全自动连续化生产防老剂rd的设备及工艺 (Equipment and process for full-automatic continuous production of antioxidant RD ) 是由 郭焕宇 刘传红 静海旺 黄启富 李品 于 2019-09-16 设计创作，主要内容包括：本发明公开了一种全自动连续化生产防老剂RD的设备及工艺,属于防老剂生产技术领域。本发明公开了一种全自动连续化生产防老剂RD的设备与工艺。该工艺采用串连釜式反应装置,以溢流的方式采出物料一步法合成防老剂RD,整个工艺过程包括成盐、缩聚、中和、分水等全部采用自动化仪表连锁控制,实现了防老剂RD生产连续进料、连续成盐、连续缩聚、连续中和、连续分水的操作,替代了目前国内普遍使用的间歇性釜式反应合成工艺。该工艺实现了连续化生产,自动化控制,可大幅度缩减岗位人员,降低员工劳动强度,同时很大程度上提高了生产及产品质量的稳定性。(The invention discloses equipment and a process for full-automatic continuous production of an antioxidant RD, and belongs to the technical field of antioxidant production. The invention discloses a full-automatic continuous production device and a process for an antioxidant RD. The process adopts a serial kettle type reaction device, materials are extracted in an overflow mode to synthesize the antioxidant RD by a one-step method, the whole process comprises salt formation, polycondensation, neutralization and water diversion which are all controlled by an automatic instrument in a linkage manner, the operations of continuous feeding, continuous salt formation, continuous polycondensation, continuous neutralization and continuous water diversion in the production of the antioxidant RD are realized, and the intermittent kettle type reaction synthesis process commonly used in China at present is replaced. The process realizes continuous production and automatic control, can greatly reduce post personnel, reduce the labor intensity of the personnel, and simultaneously improve the stability of production and product quality to a great extent.)

1. The utility model provides a full-automatic serialization production anti-aging agent RD's equipment which characterized in that: comprises a salt forming kettle, a polycondensation kettle, a buffer tank, a neutralization tank and a delayer;

the salt forming kettle is respectively connected with a aniline pump and a hydrochloric acid pump through pipelines; a hydrochloric acid feeding quantity regulating valve group is arranged on a pipeline for communicating the salt forming kettle with the hydrochloric acid pump; an aniline feeding amount adjusting valve group is arranged on a pipeline which communicates the salt forming kettle and the aniline pump;

an overflow port is arranged on the wall of the salifying kettle; the overflow port of the salt forming kettle is communicated with the polycondensation kettle through a pipeline;

the polycondensation kettle is connected with an acetone pump through a pipeline, and an acetone feeding amount adjusting valve group is arranged on the pipeline between the acetone pump and the polycondensation kettle;

an overflow port is arranged on the polycondensation kettle, and the overflow port of the polycondensation kettle is communicated with the buffer tank through a pipeline;

the bottom of the buffer tank is communicated with the neutralization tank through a pipeline; a first liquid level regulating valve group for regulating the liquid level in the buffer tank is arranged on a pipeline between the buffer tank and the neutralization tank;

the neutralization tank is respectively communicated with the liquid caustic soda tank and the delayer through pipelines; a liquid caustic soda feeding amount adjusting valve group is arranged between the neutralization tank and the liquid caustic soda tank; a second liquid level regulating valve group for regulating the liquid level in the neutralization tank is arranged on a pipeline between the neutralization tank and the delayer;

a third liquid level regulating valve group for regulating the liquid level in the delayer is arranged on a pipeline behind the delayer;

and an on-line conductivity tester is arranged in the delayer.

2. The full-automatic continuous production equipment of the antioxidant RD as claimed in claim 1, characterized in that: a polycondensation kettle circulating pipeline is also arranged outside the polycondensation kettle; one end of the polycondensation kettle circulating pipeline is arranged at the bottom of the polycondensation kettle, the other end of the polycondensation kettle circulating pipeline is arranged at the top of the polycondensation kettle, and a first circulating pump is arranged on the polycondensation kettle circulating pipeline.

3. The full-automatic continuous production equipment of the antioxidant RD as set forth in claim 1 or 2, characterized in that: a neutralization tank circulating pipeline is arranged outside the neutralization tank; one end of the neutralization tank circulating pipeline is arranged at the bottom of the neutralization tank, and the other end of the neutralization tank circulating pipeline is arranged at the top of the neutralization tank; and a second circulating pump and a static mixer are arranged on the circulating pipeline of the neutralization tank.

4. The full-automatic continuous production equipment of the antioxidant RD as claimed in claim 1, characterized in that: and a stirring device and a heating device are arranged in the salt forming kettle and the polycondensation kettle.

5. The full-automatic continuous production equipment of antioxidant RD of claim 4, characterized in that: the heating device is a steam coil.

6. The full-automatic continuous production equipment of the antioxidant RD as claimed in claim 1, characterized in that: the hydrochloric acid feeding amount adjusting valve group, the aniline feeding amount adjusting valve group and the acetone feeding amount adjusting valve group are all composed of flow meters and adjusting valves.

7. The full-automatic continuous production equipment of the antioxidant RD as claimed in claim 1, characterized in that: the liquid caustic soda feeding quantity regulating valve group consists of a flowmeter, a regulating valve and a pH on-line tester.

8. The full-automatic continuous production equipment of the antioxidant RD as claimed in claim 1, characterized in that: the first liquid level regulating valve group and the second liquid level regulating valve group are both composed of a liquid level controller and a regulating valve; the third liquid level regulating valve group consists of an electric conductivity on-line tester, a liquid level controller and a regulating valve.

9. The process for producing the antioxidant RD in a full-automatic continuous manner by adopting the equipment as claimed in claim 1, is characterized in that:

1) pumping aniline or recovered aniline and hydrochloric acid into a salt forming kettle, wherein the feeding amount is controlled by an aniline feeding amount regulating valve group and a hydrochloric acid feeding amount regulating valve group; when the salt forming material is fed to an overflow port of the salt kettle, the salt forming material automatically overflows to the polycondensation kettle;

2) pumping acetone or recovered acetone into the polycondensation kettle, adjusting the feeding amount through an acetone feeding amount adjusting valve group, participating in the polycondensation reaction, and automatically overflowing to a buffer tank when the liquid level of the polycondensation material reaches an overflow port of the polycondensation kettle;

3) the liquid level in the buffer tank is regulated by a first liquid level regulating valve group, and when the liquid level exceeds a set value, the liquid output from the buffer tank to the neutralization tank is increased; otherwise, the liquid output quantity from the buffer tank to the neutralization tank is reduced;

4) pumping the liquid caustic soda into a neutralization tank, and regulating the pumping amount of the liquid caustic soda by a liquid caustic soda feeding amount regulating valve group; pumping the neutralized material into a delayer, adjusting the liquid level in the neutralization tank through a second liquid level adjusting valve group, and increasing the liquid output from the neutralization tank to the delayer when the liquid level exceeds a set value; otherwise, the liquid output from the neutralization tank to the delaminator is reduced;

5) layering the neutralized materials in a layering device, wherein the upper oil phase is a crude product of RD, and the lower water phase is a water phase; determining a layered interface through an electric conductivity online tester; the overflow of the upper oil phase is extracted and enters the next distillation process; and extracting the lower water phase to a wastewater treatment process.

10. The fully automatic continuous process for producing the antioxidant RD as claimed in claim 9, wherein:

in the step 1), the retention time of the salifying material in a salifying kettle is 2 ~ 3 h, the molar ratio of hydrochloric acid to aniline in the salifying kettle is 0.1 ~ 0.4.4: 1, and the salifying temperature is 110 ~ 120 ℃;

in the step 2), the material retention time in the polycondensation kettle is 4 ~ 5h, the molar ratio of acetone to aniline is 5 ~ 7:1, and the polycondensation temperature is 125 ~ 135 ℃;

in the step 3), the polycondensation materials stay in a buffer tank for curing, and the stay time is 0.5 ~ 1.5.5 h;

in the step 4), a pH online tester tests the pH value of the aqueous phase mother liquor in the step 5), and the pH online tester and a liquid caustic soda feeding amount regulating valve are controlled in a linkage manner to stabilize the pH value of the aqueous phase to be 8 ~ 12;

in the step 5), the material stays in the delayer for 1 ~ 2 h, the conductivity in the delayer is converted into the interface height of the component layer in the data of the tester and is transmitted to the DCS system, and the interface height is controlled by the liquid level of the component layer and a third liquid level regulating valve group in a linkage mode.

Technical Field

The invention relates to the technical field of antioxidant production, in particular to equipment and a process for full-automatic continuous production of an antioxidant RD.

Background

The rubber antioxidant RD has the chemical name of 2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer, is a ketoamine antioxidant, has extremely strong protective effect on rubber aging caused by heat and oxygen, and is one of the varieties with the largest antioxidant yield and consumption in China.

The anti-aging agent RD is prepared by generally using aniline and acetone as raw materials and carrying out the processes of salifying, polycondensation, neutralization, distillation, granulation and the like under the action of an acid catalyst. At present, the method for producing the antioxidant RD at home and abroad mainly comprises a two-step method and a one-step method.

The two-step production process is that aniline and acetone are first condensed under the action of acid catalyst to produce monomer 2, 2, 4-trimethyl-1, 2-dihydroquine, and then the monomer is polymerized under the action of acid catalyst to produce antioxidant RD. The one-step production process is that condensation and polymerization of aniline and acetone are carried out simultaneously in the same reaction device to produce the antioxidant RD in one step.

The advantages of the one-step production process are short process route, low investment and low raw material consumption, but the content of effective bodies is lower than that of the two-step production process.

At present, most manufacturers of the anti-aging agent RD at home and abroad use a one-step synthesis route, and adopt an intermittent production method for single batch feeding. The raw materials are respectively metered and then put into a reaction kettle, then the temperature is raised for reaction, the materials are transferred to the next procedure after the reaction is finished, the neutralization procedure needs to be matched with alkali for feeding, standing and mother liquor separation, the middle part needs to be manually sampled for analyzing acidity and alkalinity, the operation is complex, the equipment utilization rate is low, and the production efficiency is low.

Disclosure of Invention

The invention provides equipment and a process for full-automatic continuous production of antioxidant RD, aiming at solving various defects of present domestic antioxidant RD production process such as intermittent production, complex operation, poor safety, low equipment utilization rate, low production efficiency, unstable product quality and the like.

The technical scheme of the invention is as follows:

a full-automatic continuous production device for an antioxidant RD comprises a salt forming kettle, a polycondensation kettle, a buffer tank, a neutralization tank and a delayer;

the salt forming kettle is respectively connected with a aniline pump and a hydrochloric acid pump through pipelines; a hydrochloric acid feeding quantity regulating valve group is arranged on a pipeline for communicating the salt forming kettle with the hydrochloric acid pump; an aniline feeding amount adjusting valve group is arranged on a pipeline which communicates the salt forming kettle and the aniline pump;

an overflow port is arranged on the wall of the salifying kettle; the overflow port of the salt forming kettle is communicated with the polycondensation kettle through a pipeline;

the polycondensation kettle is connected with an acetone pump through a pipeline, and an acetone feeding amount adjusting valve group is arranged on the pipeline between the acetone pump and the polycondensation kettle;

an overflow port is arranged on the polycondensation kettle, and the overflow port of the polycondensation kettle is communicated with the buffer tank through a pipeline;

the bottom of the buffer tank is communicated with the neutralization tank through a pipeline; a first liquid level regulating valve group for regulating the liquid level in the buffer tank is arranged on a pipeline between the buffer tank and the neutralization tank;

the neutralization tank is respectively communicated with the liquid caustic soda tank and the delayer through pipelines; a liquid caustic soda feeding amount adjusting valve group is arranged between the neutralization tank and the liquid caustic soda tank; a second liquid level regulating valve group for regulating the liquid level in the neutralization tank is arranged on a pipeline between the neutralization tank and the delayer;

a third liquid level regulating valve group for regulating the liquid level in the delayer is arranged on a pipeline behind the delayer;

and an on-line conductivity tester is arranged in the delayer.

As a preferred scheme, a polycondensation kettle circulating pipeline is also arranged outside the polycondensation kettle; one end of the polycondensation kettle circulating pipeline is arranged at the bottom of the polycondensation kettle, the other end of the polycondensation kettle circulating pipeline is arranged at the top of the polycondensation kettle, and a first circulating pump is arranged on the polycondensation kettle circulating pipeline.

Preferably, a neutralization tank circulating pipeline is arranged outside the neutralization tank; one end of the neutralization tank circulating pipeline is arranged at the bottom of the neutralization tank, and the other end of the neutralization tank circulating pipeline is arranged at the top of the neutralization tank; and a second circulating pump and a static mixer are arranged on the circulating pipeline of the neutralization tank.

As a preferred scheme, a stirring device and a heating device are arranged in the salt forming kettle and the polycondensation kettle.

Further, the heating device is a steam coil.

As a preferred scheme, the hydrochloric acid feeding amount regulating valve bank, the aniline feeding amount regulating valve bank and the acetone feeding amount regulating valve bank are all composed of flow meters and regulating valves.

As a preferred scheme, the liquid caustic soda feeding quantity regulating valve group consists of a flowmeter, a regulating valve and a pH online tester.

As a preferred scheme, the first liquid level regulating valve group and the second liquid level regulating valve group are respectively composed of a liquid level controller and a regulating valve; the third liquid level regulating valve group consists of an electric conductivity on-line tester, a liquid level controller and a regulating valve.

The method for producing the antioxidant RD in a full-automatic continuous manner by adopting the equipment comprises the following steps:

1) pumping aniline or recovered aniline and hydrochloric acid into a salt forming kettle, wherein the feeding amount is controlled by an aniline feeding amount regulating valve group and a hydrochloric acid feeding amount regulating valve group; when the salt forming material is fed to an overflow port of the salt kettle, the salt forming material automatically overflows to the polycondensation kettle;

2) pumping acetone or recovered acetone into the polycondensation kettle, adjusting the feeding amount through an acetone feeding amount adjusting valve group, participating in the polycondensation reaction, and automatically overflowing to a buffer tank when the liquid level of the polycondensation material reaches an overflow port of the polycondensation kettle;

3) the liquid level in the buffer tank is regulated by a first liquid level regulating valve group, and when the liquid level exceeds a set value, the liquid output from the buffer tank to the neutralization tank is increased; otherwise, the liquid output quantity from the buffer tank to the neutralization tank is reduced;

4) pumping the liquid caustic soda into a neutralization tank, and regulating the pumping amount of the liquid caustic soda by a liquid caustic soda feeding amount regulating valve group; pumping the neutralized material into a delayer, adjusting the liquid level in the neutralization tank through a second liquid level adjusting valve group, and increasing the liquid output from the neutralization tank to the delayer when the liquid level exceeds a set value; otherwise, the liquid output from the neutralization tank to the delaminator is reduced;

5) layering the neutralized materials in a layering device, wherein the upper oil phase is a crude product of RD, and the lower water phase is a water phase; determining a layered interface through an electric conductivity online tester; the overflow of the upper oil phase is extracted and enters the next distillation process; and extracting the lower water phase to a wastewater treatment process.

As a preferred scheme, the process for full-automatic continuous production of the antioxidant RD comprises the following steps:

in the step 1), the retention time of the salifying material in a salifying kettle is 2 ~ 3 h, the molar ratio of hydrochloric acid to aniline in the salifying kettle is 0.1 ~ 0.4.4: 1, and the salifying temperature is 110 ~ 120 ℃;

in the step 2), the material retention time in the polycondensation kettle is 4 ~ 5h, the molar ratio of acetone to aniline is 5 ~ 7:1, and the polycondensation temperature is 125 ~ 135 ℃;

in the step 3), the polycondensation materials stay in a buffer tank for curing, and the stay time is 0.5 ~ 1.5.5 h;

in the step 4), a pH online tester tests the pH value of the aqueous phase mother liquor in the step 5), and the pH online tester and a liquid caustic soda feeding amount regulating valve are controlled in a linkage manner to stabilize the pH value of the aqueous phase to be 8 ~ 12;

in the step 5), the material stays in the delayer for 1 ~ 2 h, the conductivity in the delayer is converted into the interface height of the component layer in the data of the tester and is transmitted to the DCS system, and the interface height is controlled by the liquid level of the component layer and a third liquid level regulating valve group in a linkage mode.

The anti-aging agent RD is synthesized by one-step method by adopting a serial kettle type reaction device and extracting materials in an overflow mode, the whole process comprises salt formation, polycondensation, neutralization and water diversion which are all controlled by an automatic instrument in a chain manner, the operations of continuous feeding, continuous salt formation, continuous polycondensation, continuous neutralization and continuous water diversion in the production of the anti-aging agent RD are realized, and the intermittent kettle type reaction synthesis process commonly used in China at present is replaced. The process realizes continuous production and automatic control, can greatly reduce post personnel, reduce the labor intensity of the personnel, and simultaneously improve the stability of production and product quality to a great extent.

The invention has the beneficial effects that:

1. a serial kettle type reaction device is adopted, continuous quantitative feeding is carried out, materials are extracted in an overflow mode, and the antioxidant RD is synthesized by a one-step method. The raw materials are fed stably according to a specified proportion, the retention time of salification and polycondensation is constant, the temperature is automatically controlled, and the technological parameters in the reaction process are basically unchanged.

2. The polycondensation materials adopt stirring and forced pump circulation, so that the reaction mass transfer effect is greatly improved, the reaction time is shortened, and the equipment utilization rate is improved.

3. The process realizes continuous production and DCS automatic control in the processes of feeding, salifying, polycondensation, neutralization and water diversion, can greatly reduce the number of post personnel, reduce the labor intensity of the personnel, and simultaneously improve the stability of production and product quality to a great extent.

4. The layering interface of the layering device is detected in real time by adopting an on-line conductivity detector, and signals are converted into the liquid level of the layering interface to realize remote monitoring.

5. The layered water phase (mother liquor) is detected in real time by a pH value on-line detector and is interlocked and controlled with a regulating valve for controlling the addition of liquid caustic soda, so that the materials are fully neutralized.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.

Fig. 1 is a schematic structural diagram of a full-automatic continuous production device for antioxidant RD.

Detailed Description