阅读说明：本技术 3,3′-二氯-4,4′-二氨基二苯基甲烷的连续化合成工艺 (Continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane ) 是由 高飞 郭冬冬 安星辰 侯亚军 于 2020-12-29 设计创作，主要内容包括：本发明提供了3,3’-二氯-4,4’-二氨基二苯基甲烷的连续化合成工艺,涉及化合物合成技术领域。该合成工艺包括成盐缩合、重排反应、中和分离、洗涤分液、真空干燥几个步骤。本发明通过精准调节三种原料的添加量以控制配比,实现连续化反应、后处理操作,尤其是成盐缩合步骤结合反应器的不同位置取样进行高效液相检测,及时排料至下一工序,避免出现各阶段反应体系残留及中间体发生副反应变质、产物纯度降低的现象；中和分离步骤通过过滤板对钠盐进行过滤,减少后续洗涤分液的用水量,大大节约成本；本发明实现MOCA的连续化合成,提高MOCA的合成效率和产品收率、纯度。(The invention provides a continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane, and relates to the technical field of compound synthesis. The synthesis process comprises the steps of salifying condensation, rearrangement reaction, neutralization separation, washing liquid separation and vacuum drying. According to the invention, the addition amounts of three raw materials are accurately adjusted to control the ratio, so that continuous reaction and post-treatment operation are realized, especially, the salt-forming condensation step is combined with sampling at different positions of a reactor to perform high performance liquid detection, and the materials are discharged in time to the next procedure, so that the phenomena of reaction system residue at each stage, side reaction deterioration of an intermediate and product purity reduction are avoided; in the neutralization separation step, the sodium salt is filtered by the filter plate, so that the water consumption for subsequent washing and liquid separation is reduced, and the cost is greatly saved; the invention realizes the continuous synthesis of MOCA and improves the synthesis efficiency, product yield and purity of MOCA.)

The continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane is characterized by comprising the following steps:

s1, salifying condensation: adjusting the flow rates of o-chloroaniline, formaldehyde aqueous solution and acid catalyst aqueous solution, mixing the three raw materials through a mixing pipe (64), then feeding the mixture into a reactor (12), timely sampling from a liquid phase material taking port to perform high performance liquid phase detection, and introducing salified condensation reaction liquid into a rearrangement reaction tank (2) through a material discharging pipe (16);

s2, rearrangement reaction: starting a first differential motor (22), driving a first stirring shaft (23) and stirring blades (24) to rotate by the first differential motor (22), introducing circulating water with the temperature of 75-80 ℃ into a circulating water jacket (21), and stirring the salified condensation reaction liquid by the stirring blades (24) to obtain a rearrangement reaction liquid;

s3, neutralization and separation: opening a second discharge valve (26) and a second centrifugal pump (27), enabling rearrangement reaction liquid to enter a neutralization reaction chamber (31) from a second discharge pipe (25), driving a second stirring shaft (35) and a stirring frame (36) to rotate by a second differential motor (33), adding a sodium hydroxide solution from an alkaline liquid port (34), filtering sodium salt by a filter plate (37), allowing the sodium salt to enter an oil-water separation chamber (32) for standing and layering, and allowing an oil layer to enter a washing liquid separation tank (4) through a third discharge pipe (39) under the centrifugal force of a third centrifugal pump (40);

s4, washing and separating liquid: adding water from a water adding port (41) to wash the oil layer for multiple times, discharging a water phase from a liquid discharging port (43), and discharging an oil phase into a vacuum drying tank (5) from a fourth discharging pipe (44);

s5, vacuum drying: heating the vacuum drying tank (5) in a water bath, vacuumizing the vacuum drying tank (52), and driving a spiral flood dragon (54) to rotate and stir by a third differential motor (53) to obtain a pure dried 3,3 '-dichloro-4, 4' -diaminodiphenylmethane.

2. The continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane according to claim 1, characterized in that step S1 is performed by controlling the molar ratio of o-chloroaniline, acid catalyst, formaldehyde to 1: 1.2-1.3: 0.51 to 0.53; the reactor (12) is heated to 40-45 ℃.

3. The continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane according to claim 1, characterized in that the aqueous acid catalyst solution is a 15-25 wt% aqueous hydrochloric acid solution, and the aqueous formaldehyde solution is 15-30 wt%.

4. The continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane according to claim 1, wherein the concentration of the sodium hydroxide solution in step S3 is 20 to 40 wt%, and the molar ratio of sodium hydroxide to acid catalyst is 1.1 to 1.3: 1, adjusting the pH value of the solution to 9-11 by using sodium hydroxide solution.

5. The continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane according to claim 1, wherein the number of washing times in step S4 is 3-5, and the amount of water added in each time is 0.8-1.5 times of the volume of the oil phase.

6. The continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane according to claim 1, wherein the water bath heating temperature in step S5 is 50-75 ℃, and the vacuum degree of the vacuum pump is 10-50 Pa.

Technical Field

The invention relates to the technical field of compound synthesis, in particular to a continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane.

Background

3,3 '-dichloro-4, 4' -diaminodiphenylmethane is a commonly used aromatic diamine chain extender, commonly called MOCA, can be used as a cross-linking agent and a curing agent of polyurethane, epoxy resin and the like, and a vulcanizing agent of rubber to prepare products with higher electric resistance, and is widely applied in the fields of automobiles, mechanical manufacturing, mining, sports facilities and the like.

The existing synthesis process adopts o-chloroaniline, formaldehyde and hydrochloric acid as raw materials, the o-chloroaniline reacts with the hydrochloric acid to generate o-chloroaniline hydrochloride, then the o-chloroaniline hydrochloride reacts with the formaldehyde to generate MOCA hydrochloride, the hydrochloric acid is neutralized by liquid caustic soda, and the product MOCA is obtained through the steps of water washing and the like.

The existing synthesis process cannot detect discharge materials in time during salification condensation reaction, can cause generation of byproducts, and sodium salt is not filtered in advance after neutralization reaction, so that water consumption in a washing step is increased, cost is increased, and further improvement is needed.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane.

The invention solves the technical problems through the following technical means:

the continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane includes the following steps:

s1, salifying condensation: adjusting the flow rates of o-chloroaniline, formaldehyde aqueous solution and acid catalyst aqueous solution, mixing the three raw materials through a mixing pipe, then feeding the mixture into a reactor, timely sampling from a liquid phase material taking port to perform high performance liquid phase detection, and feeding a salified condensation reaction solution into a rearrangement reaction tank through a material discharging pipe;

s2, rearrangement reaction: starting a first differential motor, driving a first stirring shaft and stirring blades to rotate by the first differential motor, introducing circulating water at 75-80 ℃ into a circulating water jacket, and stirring the salifying condensation reaction liquid by the stirring blades to obtain a rearrangement reaction liquid;

s3, neutralization and separation: opening a second discharge valve and a second centrifugal pump, allowing rearranged reaction liquid to enter a neutralization reaction chamber from a second discharge pipe, driving a second stirring shaft and a stirring frame to rotate by a second differential motor, adding a sodium hydroxide solution from an alkali liquor port, filtering sodium salt by a filter plate, allowing the rearranged reaction liquid to enter an oil-water separation chamber for standing and layering, and allowing an oil layer to enter a washing liquid separation tank through a third discharge pipe under the centrifugal force of a third centrifugal pump;

s4, washing and separating liquid: adding water from a water filling port to wash the oil layer for multiple times, discharging the water phase from a liquid outlet, and discharging the oil phase into a vacuum drying tank from a fourth discharge pipe;

s5, vacuum drying: and heating the vacuum drying tank in a water bath, vacuumizing the vacuum drying tank, and driving a spiral flood dragon to rotate and stir by using a third differential motor to obtain a pure dried 3,3 '-dichloro-4, 4' -diaminodiphenylmethane.

The synthetic process route of the invention is the same as the prior art, and the chemical reaction formula is as follows:

1) salifying condensation reaction:

2) rearrangement reaction:

3) and (3) neutralization reaction:

as a further improvement of the present invention, step S1 is to control the molar ratio of o-chloroaniline, acid catalyst, formaldehyde to be 1: 1.2-1.3: 0.51 to 0.53; the reactor is heated to 40-45 ℃.

As a further improvement of the invention, the aqueous acid catalyst solution is a hydrochloric acid solution with the concentration of 15-25 wt%, and the concentration of the aqueous formaldehyde solution is 15-30 wt%.

As a further improvement scheme of the invention, the concentration of the sodium hydroxide solution in the step S3 is 20-40 wt%, and the molar ratio of the sodium hydroxide to the acid catalyst is 1.1-1.3: 1, adjusting the pH value of the solution to 9-11 by using sodium hydroxide solution.

As a further improved scheme of the invention, the number of times of washing in the step S4 is 3-5, and the water addition amount is 0.8-1.5 times of the volume of the oil phase.

As a further improved scheme of the invention, the water bath heating temperature of the step S5 is 50-75 ℃, and the vacuum degree of the vacuum pump is 10-50 Pa.

The invention has the beneficial effects that:

according to the continuous synthesis process of the 3,3 '-dichloro-4, 4' -diaminodiphenylmethane, the addition amounts of the three raw materials are accurately adjusted to control the proportion, so that continuous reaction and post-treatment operations of salifying condensation, rearrangement, neutralization and pH adjustment, oil-water separation, oil layer washing and dehydration drying are realized, particularly, the salifying condensation step is combined with sampling at different positions of a reactor to perform high-efficiency liquid phase detection, and the materials are discharged to the next procedure in time, so that the phenomena of reaction system residue at each stage, side reaction deterioration of an intermediate and product purity reduction are avoided; in the neutralization separation step, the sodium salt is filtered by the filter plate, so that the water consumption for subsequent washing and liquid separation is reduced, and the cost is greatly saved; the invention realizes the continuous synthesis of MOCA and improves the synthesis efficiency, product yield and purity of MOCA.

Drawings

FIG. 1 is a schematic structural view of a continuous synthesis system for 3,3 '-dichloro-4, 4' -diaminodiphenylmethane in example 3 of the present invention.

FIG. 2 is a schematic structural view of a charging system according to an embodiment of the present invention.

In the figure: 1. a salifying condensation tank; 2. a rearrangement reaction tank; 3. a neutralization separation tank; 4. washing liquid separation tank; 5. a vacuum drying tank; 6. an o-chloroaniline feeding tank; 7. a formaldehyde aqueous solution tank; 8. an acid catalyst tank; 11. a heat-preserving jacket; 12. a reactor; 13. a discharge pipe; 14. a first discharge valve; 15. a first centrifugal pump; 16. a discharge pipe; 17. heating wires; 21. a circulating water jacket; 22. a first differential motor; 23. a first stirring shaft; 24. stirring blades; 25. a second discharge pipe; 26. a second discharge valve; 27. a second centrifugal pump; 31. a reaction chamber; 32. an oil-water separation chamber; 33. a second differential motor; 34. an alkaline solution port; 35. a second stirring shaft; 36. a stirring frame; 37. a filter plate; 38. a third discharge valve; 39. a third discharge pipe; 40. a third centrifugal pump; 41. a water filling port; 42. an anti-adhesion plate; 43. a liquid discharge port; 44. a fourth discharge pipe; 45. a fourth centrifugal pump; 51. a vacuum tube; 52. a vacuum pump; 53. a third differential motor; 54. a spiral flood dragon; 61. a first feed tube; 62. a first charging valve; 63. a first metering pump; 64. a mixing pipe; 71. a second feed tube; 72. a second charging valve; 73. a second metering pump; 81. a third feed tube; 82. a third charging valve; 83. and a third metering pump.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.

Example 1

As shown in fig. 1-2, this example provides a continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane, including the following steps:

s1, salifying condensation: opening a first feeding valve 62 and a first metering pump 63, and adjusting the flow of the raw material o-chloroaniline in the o-chloroaniline feeding tank 6 through a first feeding pipe 61; opening a second feeding valve 72 and a second metering pump 73, and adjusting the flow rate of the formaldehyde water solution in the formaldehyde water solution tank 7 through a second feeding pipe 71; and opening a third charging valve 82 and a third metering pump 83, accurately adjusting the flow of the acid catalyst in the acid catalyst tank 8 through a third charging pipe 81, and controlling the molar ratio of the o-chloroaniline, the acid catalyst and the formaldehyde to be 1: 1.2-1.3: 0.51-0.53, mixing the three raw materials through a mixing pipe 64, then feeding the mixture into a reactor 12 of a salt-forming condensation tank 1, heating the reactor 12 to 42 ℃ by a heating wire 17, sampling in time from a liquid-phase material taking port to perform high-efficiency liquid-phase detection, judging whether the raw materials are completely reacted and whether byproducts are generated, opening a first discharging valve 14 and a first centrifugal pump 15 in time, and feeding the salt-forming condensation reaction liquid with high product purity into a rearrangement reaction tank 2 from a material discharging pipe 16; wherein the acid catalyst aqueous solution is a hydrochloric acid aqueous solution with the concentration of 15-25 wt%, and the formaldehyde aqueous solution with the concentration of 15-30 wt%.

S2, rearrangement reaction: starting a first differential motor 22, driving a first stirring shaft 23 and stirring blades 24 to rotate by the first differential motor 22, introducing circulating water with the temperature of 75-80 ℃ into a circulating water jacket 21, and stirring the salifying condensation reaction liquid by the stirring blades 24 to obtain a rearrangement reaction liquid;

s3, neutralization and separation: opening a second discharge valve 26 and a second centrifugal pump 27, enabling rearranged reaction liquid to enter a neutralization reaction chamber 31 from a second discharge pipe 25, driving a second stirring shaft 35 and a stirring frame 36 to rotate by a second differential motor 33, adding a sodium hydroxide solution from an alkali liquor port 34, enabling the stirring frame 36 to rotate, promoting a neutralization reaction to obtain neutralized reaction liquid, filtering sodium salt by a filter plate 37, allowing the sodium salt to enter an oil-water separation chamber 32 for standing and layering, and allowing an oil layer to enter a washing liquid separation tank 4 through a third discharge pipe 39 under the centrifugal force of a third centrifugal pump 40; wherein the concentration of the sodium hydroxide solution is 20-40 wt%, and the molar ratio of the sodium hydroxide to the acid catalyst is 1.1-1.3: 1, adjusting the pH value to 9-11 by using a sodium hydroxide solution;

s4, washing and separating liquid: adding water from a water adding port 41, washing the oil layer for multiple times, discharging the water phase from a liquid discharge port 43, and discharging the oil phase into the vacuum drying tank 5 from a fourth discharge pipe 44; wherein, the times of washing for many times are 3-5 times, and the water addition amount is 0.8-1.5 times of the volume of the oil phase each time;

s5, vacuum drying: and heating the vacuum drying tank 5 in a water bath, driving a spiral flood dragon 54 to rotate by a third differential motor 53, so that low-boiling components and moisture are gasified and then sucked away by a vacuum pump 52, and obtaining a pure dry 3,3 '-dichloro-4, 4' -diaminodiphenylmethane. Wherein the temperature of the water bath heating is 50-75 ℃, and the vacuum degree of the vacuum pump is 10-50 Pa.

The continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane of this example, on the basis of the prior art, through the addition of accurate three kinds of raw materialss of regulation with control ratio, realize salifying condensation, the rearrangement, neutralization regulation pH, water oil separating, oil reservoir washing, dehydration drying's serialization reaction, the aftertreatment operation, especially salifying condensation step combines the different positions sample of reactor to carry out high performance liquid phase and detects, in time arrange material to next process, the phenomenon that each stage reaction system remains and the midbody takes place the side reaction and is rotten, product purity reduces, neutralization separation step filters the sodium salt through the filter, reduce the water consumption of follow-up washing branch liquid, the cost is greatly saved, this embodiment realizes MOCA's serialization synthesis, the synthetic efficiency and the product yield of MOCA, purity are improved.

Example 2

As shown in FIGS. 1-2, in this example, in the range of example 1, the molar ratio of o-chloroaniline, hydrochloric acid and formaldehyde was controlled to be 1: 1.22: 0.53, heating the reactor 12 to 40 ℃ by a heating wire 17, wherein the addition amount of the o-chloroaniline is 10kg, the concentration of the hydrochloric acid aqueous solution is 20 wt%, and the concentration of the formaldehyde aqueous solution is 22 wt%; circulating water with the temperature of 75 ℃ is introduced for rearrangement reaction; the concentration of the sodium hydroxide solution in the neutralization separation step was 26 wt%, and the molar ratio of sodium hydroxide to acid catalyst was 1.2: 1, adjusting the pH value to 10 by using a sodium hydroxide solution; the washing times of the washing and liquid separating steps are 3 times, and the water adding amount is 1.2 times of the volume of the oil phase each time; the water bath heating temperature of the vacuum drying step is 65 ℃, and the vacuum degree is 20 Pa.

This example was prepared to give 8527.1g of product in 95.7% yield and 95.6% purity by HPLC.

Example 3

As shown in FIGS. 1-2, in this example, in the range of example 1, the molar ratio of o-chloroaniline, hydrochloric acid and formaldehyde was controlled to be 1: 1.25: 0.52, heating the reactor 12 to 44 ℃ by a heating wire 17, wherein the addition amount of the o-chloroaniline is 10kg, the concentration of the hydrochloric acid aqueous solution is 22 wt%, and the concentration of the formaldehyde aqueous solution is 25 wt%; circulating water with the temperature of 77 ℃ is introduced for rearrangement reaction; the concentration of the sodium hydroxide solution in the neutralization separation step was 30 wt%, and the molar ratio of sodium hydroxide to acid catalyst was 1.25: 1, adjusting the pH value to 9.5 by using a sodium hydroxide solution; the washing times of the washing and liquid separating steps are 4 times, and the water adding amount is 1 time of the volume of the oil phase each time; the water bath heating temperature of the vacuum drying step is 60 ℃, and the vacuum degree is 15 Pa.

This example was prepared to give 8562.7g of product in 96.1% yield with 94.8% purity by HPLC.

Example 4

As shown in FIGS. 1-2, in this example, in the range of example 1, the molar ratio of o-chloroaniline, hydrochloric acid and formaldehyde was controlled to be 1: 1.26: 0.51, heating the reactor 12 to 43 ℃ by a heating wire 17, wherein the addition amount of the o-chloroaniline is 10kg, the concentration of the hydrochloric acid aqueous solution is 18 wt%, and the concentration of the formaldehyde aqueous solution is 25 wt%; circulating water with the temperature of 73 ℃ is introduced for rearrangement reaction; the concentration of the sodium hydroxide solution in the neutralization separation step was 35 wt%, and the molar ratio of sodium hydroxide to acid catalyst was 1.3: 1, adjusting the pH value to 11 by using a sodium hydroxide solution; the washing times of the washing and liquid separating steps are 5 times, and the water adding amount is 0.9 time of the volume of the oil phase each time; the water bath heating temperature in the vacuum drying step is 70 ℃, and the vacuum degree is 30 Pa.

This example was prepared to give 8580.6g of product in 96.3% yield with 94.5% purity by HPLC.

Example 5

As shown in fig. 1-2, this example provides a continuous synthesis system of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane, which is suitable for the continuous synthesis process of 3,3 '-dichloro-4, 4' -diaminodiphenylmethane described above, and includes a feeding system, a salifying condensation tank 1, a rearrangement reaction tank 2, a neutralization separation tank 3, a washing separation tank 4, and a vacuum drying tank 5.

The feeding system is used for respectively adjusting the adding amounts of the raw materials of o-chloroaniline, formaldehyde aqueous solution and acid catalyst and mixing the three raw materials, and comprises an o-chloroaniline feeding tank 6, a formaldehyde aqueous solution tank 7 and an acid catalyst tank 8; the salifying condensation tank 1 is used for reacting o-chloroaniline with hydrochloric acid to generate o-chloroaniline hydrochloride, and then continuing to condense with formaldehyde to generate an MOCA intermediate; the rearrangement reaction tank 2 is used for rearranging the MOCA intermediate to generate MOCA hydrochloride; the neutralization separation tank 3 is used for reacting MOCA hydrochloride with a sodium hydroxide solution to generate MOCA, sodium chloride and water, filtering and performing oil-water separation to obtain an oil layer and a water layer; the washing liquid separation tank 4 is used for adding water to wash and separate liquid from the oil layer; and the vacuum drying tank 5 is used for vacuumizing the oil layer containing the MOCA, and then stirring and drying to obtain a MOCA pure product.

The continuous synthesis system of the embodiment can realize continuous reaction and post-treatment operations of salifying condensation, rearrangement, pH regulation by neutralization, oil-water separation, oil layer washing, dehydration and drying, avoids the phenomena of reaction system residue at each stage, side reaction deterioration of intermediates and low product purity, realizes continuous synthesis of MOCA, and improves synthesis efficiency, product yield and purity of MOCA.

Specifically, a first feeding pipe 61 is arranged at the bottom of the o-chloroaniline feeding tank 6, and a first feeding valve 62 and a first metering pump 63 are sequentially arranged on the first feeding pipe 61; the bottom of the formaldehyde water solution tank 7 is provided with a second feeding pipe 71, and a second feeding valve 72 and a second metering pump 73 are sequentially arranged on the second feeding pipe 71; the bottom of the acid catalyst tank 8 is provided with a third feeding pipe 81, and the third feeding pipe 81 is sequentially provided with a third feeding valve 82 and a third metering pump 83; the tail ends of the first feeding pipe 61, the second feeding pipe 71 and the third feeding pipe 81 are communicated with the mixing pipe 64. The flow of the raw material o-chloroaniline in the o-chloroaniline feeding tank 6 through the first feeding pipe 61 is accurately adjusted by adjusting the first feeding valve 62 and the first metering pump 63; the flow of the aqueous formaldehyde solution in the aqueous formaldehyde solution tank 7 through the second feeding pipe 71 is accurately adjusted by adjusting the second feeding valve 72 and the second metering pump 73; through adjusting third filling valve 82 and third metering pump 83, the accurate flow of adjusting the acid catalyst in acid catalyst jar 8 through third filling tube 81 realizes the ratio accurate regulation of three kinds of raw materialss.

Salify condensation jar 1 includes that heat preservation presss from both sides cover 11, be equipped with reactor 12 in the heat preservation presss from both sides the cover 11, reactor 12 is the heliciform from the top down, outwards extend a plurality of first discharging pipes 13 on reactor 12, reactor 12's peripheral parcel has heater strip 17, be equipped with first bleeder valve 14 on the first discharging pipe 13 in proper order, first centrifugal pump 15, the end-to-end connection of first discharging pipe 13 has the row of material pipe 16 with rearrangement retort 2 top intercommunication, all be equipped with the liquid phase on every first discharging pipe 13 and get the material mouth. Heat dissipation in the heat preservation jacket 11 has slowed down reactor 12, spiral helicine reactor 12 has increased the area of contact of three kinds of raw materials, the heater strip 17 of parcel has increased the heating area of reaction mixture, the reaction rate of salify condensation has been improved, a plurality of first discharging pipe 13's design simultaneously, the convenient material mouth of getting from the liquid phase in time takes a sample and carries out high performance liquid phase and detects, judge whether the raw materials reacts completely, whether have the accessory substance to produce, and in time open first bleeder valve 14 and first centrifugal pump 15, arrange into rearrangement reaction in 16 rearrangement retort 2 with the salify condensation reaction liquid that the product purity is high from arranging material pipe.

Rearrangement retort 2 includes that circulating water presss from both sides the cover 21, and circulating water presss from both sides the top of cover 21 and is equipped with first differential motor 22, and the motor shaft of first differential motor 22 is connected with the first (mixing) shaft 23 that stretches into in rearrangement retort 2, and the periphery of first (mixing) shaft 23 is equipped with stirring leaf 24, and rearrangement retort 2's bottom is equipped with the second discharging pipe 25 with 3 top intercommunications of neutralization knockout drum, is equipped with second bleeder valve 26 and second centrifugal pump 27 on the second discharging pipe 25. After the salt-forming condensation reaction liquid is introduced into the rearrangement reaction tank 2, the first differential motor 22 is started, the first stirring shaft 23 and the stirring blades 24 are driven by the first differential motor 22 to rotate, the circulating warm water is introduced into the circulating water jacket 21, and the stirring blades 24 stir the salt-forming condensation reaction liquid to promote the rearrangement reaction to obtain the rearrangement reaction liquid.

The neutralization separation tank 3 comprises a neutralization reaction chamber 31 arranged from top to bottom, an oil-water separation chamber 32, the top of the neutralization reaction chamber 31 is provided with a second differential motor 33 and an alkali liquor port 34, the motor shaft of the second differential motor 33 is connected with a second stirring shaft 35 extending into the neutralization reaction chamber 31, the periphery of the second stirring shaft 35 is provided with a stirring frame 36, the bottom of the neutralization reaction chamber 31 is provided with a filtering plate 37, the bottom of the filtering plate 37 is provided with a third discharge valve 38, the bottom side wall of the oil-water separation chamber 32 is provided with a third discharge pipe 39 connected with the top of the washing liquid separation tank 4, and the third discharge pipe 39 is provided with a third centrifugal pump 40. After the rearranged reaction liquid enters the neutralization reaction chamber 31 from the second discharge pipe 25, the second differential motor 33 drives the second stirring shaft 35 and the stirring frame 36 to rotate, sodium hydroxide solution is added from the alkali liquor port 34, the stirring frame 36 rotates to promote the neutralization reaction to obtain neutralized reaction liquid, and the filtering plate 37 filters sodium salt and then enters the oil-water separation chamber 32 to stand and layer; the stirring frame 36 rotates to accelerate the dissipation of neutralization reaction heat and increase the contact area of sodium hydroxide and hydrochloric acid; the filter plate 37 filters and removes most of sodium salt to obtain neutralization and desalination reaction liquid, so that the water consumption for subsequent water washing is reduced, and the cost is saved.

The top of the washing liquid separating tank 4 is provided with a water filling port 41, the tank body is internally provided with a plurality of anti-adhesion plates 42, the bottom of the washing liquid separating tank 4 is provided with a liquid outlet 43, the side part of the liquid outlet 43 is connected with a fourth discharging pipe 44 communicated with the top of the vacuum drying tank 5, and the fourth discharging pipe 44 is provided with a fourth centrifugal pump 45. The anti-sticking plate 42 is inclined downward toward the center of the washing component liquid tank 4. After water is added from the water adding port 41, the neutralization and desalination reaction liquid is washed for a plurality of times, the water phase is discharged from the liquid discharge port 43, and the oil phase is discharged from the fourth discharge pipe 44 into the vacuum drying tank 5 for vacuum drying.

The top of vacuum drying jar 5 is connected with vacuum pump 52 through vacuum tube 51, and the lateral wall is equipped with third differential motor 53, and the motor shaft of third differential motor 53 is connected with the spiral flood dragon 54 that the level runs through vacuum drying jar 5. After the oil phase enters the vacuum drying tank 5, the vacuum drying tank 5 is heated in a water bath, the third differential motor 53 drives the spiral flood dragon 54 to rotate, so that low-boiling components and moisture are gasified and then sucked away by the vacuum pump 52, the spiral flood dragon 54 promotes dispersion and heat exchange of products, drying efficiency is improved, and a dried pure product is obtained.

It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.

The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.