Screw continuous washing apparatus, method of washing solid and polyarylene sulfide

Abstract

The present application belongs to the technical field of washing equipment and washing method, and particularly relates to a spiral continuous washing equipment and a washing method of solid and polyarylene sulfide, wherein the spiral continuous washing equipment is provided with a vertical washing main body and at least one spiral channel for contacting the material to be washed with washing liquid, and the spiral channel is fixedly arranged in the vertical washing main body from top to bottom. The vertical washing main body is provided with a settling cavity and a washing cavity, the settling cavity is arranged above the washing cavity, and the spiral channel is fixedly arranged in the washing cavity from top to bottom. The washing cavity is divided into at least two washing chambers from top to bottom, each of the washing chambers is provided with a liquid inlet of the washing liquid, and the spiral channel passes through all the washing chambers. The equipment has no dead angle, so that the material to be washed does not accumulate in the flowing process, the residence time of the material is increased, the washing efficiency is improved through multiple washing of the washing liquid, and the material to be washed can flow downward automatically, thereby reducing energy consumption.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of washing equipment and washing method, and particularly relates to a spiral continuous washing equipment, a solid washing method and a polyarylene sulfide washing method. BACKGROUND

[0002] In the field of chemical industry, solid washing refers to washing the solid by liquid contact to remove impurities such as raw materials, by-products and the like attached to or wrapped in the solid after the raw materials go through a series of reactions. Polyarylene sulfide (PAS for short) represented by polyphenylene sulfide is an engineering plastic with excellent heat resistance, chemical resistance, flame resistance, mechanical strength, electrical properties and dimensional stability, and is a common industrial solid. PAS can be used in a wide range of technical fields such as electrical instruments, electronic instruments, automotive instruments and packaging materials by general melt processing methods such as extrusion molding, injection molding and compression molding to produce various molded products, films, sheets and fibers. The PAS preparation method mainly comprises reacting a sulfur source and a dihalogen aromatic compound such as p-dichlorobenzene (pDCB for short) in an organic amide solvent such as N-methylpyrrolidone (NMP for short) under heating. The sulfur source is generally an alkali metal sulfide, an alkali metal hydrosulfide or a mixture thereof. When an alkali metal hydrosulfide is used as the sulfur source, the alkali metal hydrosulfide is used in combination with an alkali metal hydroxide. The polymerization reaction of the sulfur source and the dihalogen aromatic compound is a desalting polycondensation reaction, and a large amount of salts such as NaCl (i.e. alkali metal halides) is generated after the reaction. Because the raw material contains sulfur compounds, a by-product hydrogen sulfide is generated. Therefore, after the PAS particles generated by the polymerization reaction are separated from the reaction solution and recovered, the PAS particles are put into a solid-liquid contact device, and water, an organic solvent or water and an organic solvent are used as the washing agent to wash the PAS particles to remove the NMP solution.

[0003] At present, various solid-liquid contact devices are generally required for solid washing, and there are two ways of batch washing and continuous washing for solid washing in industry. In batch washing, the material to be washed is gathered into one or multiple streams and enters a washing tank filled with washing liquid for multiple rinsing until the standard is met. This method has the advantages of stable washing effect, simple equipment and easy operation, but has the problems of difficult subsequent treatment of a large amount of washing liquid and large equipment size and large occupied area. In continuous washing, the material to be washed is gathered into one stream, which can reduce the amount of washing liquid, but also has the defect of large occupied area.

[0004] CN102424418A discloses a method for continuous filtration and washing of hydrated titanium dioxide, which is washed by using a filtration and washing device formed by connecting multiple continuous filtration and washing devices in series, and the washing water is only added in the last continuous filtration and washing device. Although the use amount of the washing liquid is reduced, multiple sets of filtration and washing devices are connected in series and a horizontal washing device is used, thereby increasing the land application area cost.

[0005] CN108219135A discloses a continuous washing device for polyphenylene sulfide resin, which comprises a feeding mechanism, a washing mechanism and a spiral stirring paddle. The washing mechanism comprises an inclined horizontal cylinder and a vertical cylinder connected thereto. The continuous washing device uses a horizontal cylinder and a vertical cylinder, and also has the problem of large land application area. Moreover, the continuous washing device uses a spiral stirring paddle as the main power to drive the polyphenylene sulfide resin to flow, and thus has the defects of high power requirement and excessive energy consumption.

[0006] CN102781568A discloses a tower type solid-liquid countercurrent contact device, a solid particle washing device and a method. The countercurrent contact device is vertically arranged to reduce the land application area. However, the countercurrent contact device is provided with multiple annular partitions in the tower main body to increase the residence time of the solid material in the tower main body and the solid-liquid contact time. However, the annular partitions cause accumulation dead angles, thereby causing the accumulation of solid particles and reducing the washing efficiency. SUMMARY

[0007] The present application provides a spiral continuous washing device without accumulation dead angles, a solid washing method and a polyarylene sulfide washing method to solve the problems in the prior art. The spiral continuous washing device has no dead angles in the interior, so that the to-be-washed material does not accumulate during the flow process, the residence time of the material is increased, the to-be-washed material is washed multiple times by the washing liquid fed through multiple stages, and the washing efficiency is improved. The to-be-washed material can flow downward autonomously, thereby reducing the energy consumption.

[0008] To achieve the above object, the technical scheme adopted by the present application is as follows:

[0009] A spiral continuous washing device is provided with a vertical washing main body and at least one spiral channel for contacting the to-be-washed material with the washing liquid. The spiral channel is fixedly arranged in the interior of the vertical washing main body from top to bottom. Preferably, the surface of the spiral channel is smooth, and preferably, the spiral channel is a double spiral channel.

[0010] The vertical washing main body is provided with a settling chamber and a washing chamber. The settling chamber is arranged above the washing chamber, and the spiral channel is fixedly arranged in the interior of the washing chamber.

[0011] The washing cavity is divided into at least two washing chambers from top to bottom, each of which is provided with a liquid inlet of washing liquid, and the spiral channel passes through all the washing chambers, preferably three, and the three washing chambers are sequentially defined as a first-stage washing chamber, a second-stage washing chamber and a third-stage washing chamber from top to bottom.

[0012] The spiral continuous washing equipment also comprises a feed disperser for dispersing the material to be washed and a liquid disperser for dispersing the washing liquid, the feed disperser is arranged in the interior of the settling cavity, and the liquid disperser is arranged in the interior of the washing cavity and one liquid disperser is arranged in each washing chamber.

[0013] The feed disperser serves as a feed inlet of the material to be washed of the vertical washing body.

[0014] The liquid disperser serves as a liquid inlet of the material to be washed of the vertical washing body.

[0015] The discharge outlet of the vertical washing body is located at the bottom of the washing cavity.

[0016] The liquid outlet of the vertical washing body is located at the sidewall of the settling cavity.

[0017] The feed disperser and the liquid disperser are both annular structures, and the surface of the annular structure is provided with a plurality of through holes, and the annular structure is preferably arranged around the outer periphery of the stirrer of the vertical washing body.

[0018] The central axis of the spiral channel is provided with a hollow stirring channel for accommodating a stirrer.

[0019] The stirrer is provided with a stirring shaft, a plurality of middle stirring paddles and a bottom stirring paddle, the middle stirring paddles and the bottom stirring paddle are fixedly arranged on the stirring shaft, the stirring shaft is fixedly arranged in the interior of the vertical washing body, and the stirring shaft is located in the stirring channel.

[0020] At least one middle stirring paddle is arranged in the range of each washing chamber, and the bottom stirring paddle is arranged at the bottom of the washing cavity.

[0021] The rotation direction of the middle stirring paddle is opposite to the rotation direction of the spiral channel.

[0022] The middle stirring paddle is a straight-blade stirring paddle, an inclined-blade stirring paddle, a propeller stirring paddle or a turbine stirring paddle, and is preferably an upward-turning stirring paddle.

[0023] The bottom stirring paddle is a straight-blade stirring paddle, an inclined-blade stirring paddle, a propeller stirring paddle or a turbine stirring paddle, and is preferably a disc turbine stirring paddle and a propeller stirring paddle.

[0024] The outer diameter of the middle stirring paddle is defined as D1, and the maximum inner diameter of the stirring channel is defined as D2, and there is 0.60D2≤D1≤0.95D2; preferably 0.70D2≤D1≤0.90D2.

[0025] The outer diameter of the bottom stirring paddle is defined as D3, and the maximum inner diameter of the washing cavity is defined as D4, and there is 0.4D4≤D2≤0.95D4; preferably 0.5D4≤D2≤0.90D4.

[0026] The diameter of the spiral channel is defined as D5, and the pitch of the spiral channel is defined as D6, and there is D5:D6=0.9-1.8; preferably D5:D6=1.0-1.5.

[0027] The opening rate of the ring structure is 15%-90%; preferably 20%-85%, and most preferably 80%.

[0028] The bottom of the settling cavity is in a funnel structure.

[0029] The bottom of the washing cavity is in a funnel structure.

[0030] The application also provides a solid washing method using the spiral continuous washing device.

[0031] In the solid washing method, the washing liquid is divided into multiple streams and enters each washing chamber through the liquid inlet, the solid particle slurry to be washed enters through the material inlet, the solid particle slurry to be washed flows through each washing chamber along the spiral channel, the washing liquid flows from bottom to top, the solid particle slurry to be washed and the washing liquid counterflow contact, and finally the washing liquid is discharged from the liquid outlet and the washed solid particles are discharged from the material outlet.

[0032] The application also provides a polyarylene sulfide washing method using the spiral continuous washing device.

[0033] In the polyarylene sulfide washing method, at room temperature and normal pressure, the washing liquid is divided into multiple streams and enters each washing chamber through the liquid inlet, the polyarylene sulfide slurry to be washed enters through the material inlet, the polyarylene sulfide to be washed flows through each washing chamber along the spiral channel, the washing liquid flows from bottom to top, the polyarylene sulfide to be washed and the washing liquid counterflow contact, and finally the washing liquid is discharged from the liquid outlet and the washed polyarylene sulfide is discharged from the material outlet.

[0034] Preferably, the solid content of the polyarylene sulfide slurry to be washed is 10%-50%; preferably 20%-40%.

[0035] Preferably, the washing liquid is an acetone solution with a concentration of 90%-100%; preferably the concentration is 95%.

[0036] Compared with the prior art, the present application has the following beneficial effects:

[0037] (1) The spiral channel of the spiral continuous washing equipment is directly fixed in the interior of the vertical washing main body, and the spiral channel does not have energy consumption problem, and the spiral channel increases the distance of the material to be washed in the washing equipment, so that the contact time with the washing liquid is increased;

[0038] (2) The spiral channel of the spiral continuous washing equipment does not have dead angle, and the material cannot be accumulated in the interior, so that the washing efficiency is improved;

[0039] (3) The present application is an integrated vertical spiral continuous washing equipment, which can greatly reduce the floor area of the equipment.

[0040] (4) The spiral continuous washing equipment divides the washing liquid into multiple strands, which respectively enters different washing cavities, forms a multi-stage washing effect, and can fully wash the material under a small amount of washing liquid. BRIEF DESCRIPTION OF DRAWINGS

[0041] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings needed to be used in the embodiment description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0042] Figure 1 The structure schematic view of the spiral continuous washing equipment of the embodiment 1.

[0043] Figure 2 The structure schematic view of the spiral continuous washing equipment of the embodiment 3.

[0044] In the drawings, the component list represented by each number is as follows:

[0045] Spiral channel 100, settling cavity 200, washing cavity 300, washing chamber 310, feeding disperser 400, liquid inlet disperser 500, discharge port 600, liquid outlet 700, agitator 800, middle stirring paddle 810, bottom stirring paddle 820. DETAILED DESCRIPTION

[0046] For the personnel in the art to better understand the technical solutions of the present application, the technical solutions of the present application are described clearly and completely below in combination with the drawings of the present application. Based on the embodiments in the present application, other similar embodiments obtained by the personnel in the art without making creative efforts should all belong to the protection scope of the present application. In addition, the direction words mentioned in the following embodiments, such as “up”, “down”, “left”, “right” and the like are only the directions of the drawings, therefore, the direction words used are used for illustration but not for limiting the present application.

[0047] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.

[0048] As used herein, the singular forms “a”, “an” and “the” include plural referents unless the context clearly dictates otherwise. It should also be understood that the term “comprising” or “having” etc. specifies the presence of stated features, integers, steps, operations, components, parts, or combinations thereof, but does not preclude the presence or addition of one or more other features, integers, steps, operations, components, parts, or combinations thereof.

[0049] It is worth mentioning that the raw materials used in the present application are all ordinary commercially available products, and their sources are not specifically limited.

[0050] Example 1

[0051] A spiral continuous washing device, as shown in Figure 1 is provided with a vertical washing main body, at least one spiral channel 100 for contacting the material to be washed with the washing liquid and an agitator 800, and the spiral channel 100 is fixedly assembled in the inside of the vertical washing main body from top to bottom. The spiral channel 100 of the present embodiment is two in particular, and the double spiral channels 100 are staggered and assembled from top to bottom.

[0052] The spiral channel 100 of the present application is provided with a hollow stirring channel in the axis, and the stirring channel is used for accommodating the agitator 800.

[0053] It should be noted that, in the normal use of the spiral continuous washing device, the ground direction is defined as the lower side. The spiral channel 100 of the present application has the effect of not producing dead angles and plays the role of a slide for the material to be washed, guiding the material to be washed to flow autonomously from top to bottom. The surface of the spiral channel 100 is smooth, reducing the static friction of the material to be washed. Moreover, the spiral channel 100 increases the flow path of the material to be washed inside the spiral continuous washing device, thus increasing the contact time of the washing liquid and improving the cleaning effect.

[0054] The spiral channel 100 of the present application is fixed inside the vertical washing main body, and the stirrer 800 is located in the stirring channel of the spiral channel 100. Therefore, the cross-sectional area of the stirrer 800 occupies a small proportion of the cross-sectional area of the vertical washing main body, the shaft power of the stirrer 800 is small, and the energy consumption is low.

[0055] The vertical washing main body of the present application is provided with a settling chamber 200 and a washing chamber 300. The settling chamber 200 is assembled above the washing chamber 300, and the spiral channel 100 is fixedly assembled inside the washing chamber 300. The bottom of the settling chamber 200 is in a funnel-shaped structure, and the bottom of the washing chamber 300 is also in a funnel-shaped structure. It should be noted that the funnel-shaped structure of the present application has the effect of preventing the bridging phenomenon of particles at the junction.

[0056] The washing chamber 300 is divided into at least two washing rooms 310 from top to bottom. Each washing room 310 is provided with a liquid inlet of washing liquid, and the spiral channel 100 passes through all the washing rooms 310.

[0057] It should be noted that the division of the washing room 310 of the present application includes but is not limited to the following: 1. The total length of the washing chamber 300 is evenly divided into corresponding segments according to the number of washing rooms 310, and each segment of the washing chamber 300 is a washing room 310; 2. According to the total length of the spiral channel 100, the number of washing rooms 310 is evenly divided into corresponding segments, and the region of the washing chamber 300 corresponding to the length of each segment of the spiral channel 100 is a washing room 310. The washing room 310 of the present embodiment is divided according to the second method. It should be noted that the number of washing rooms 310 of the present application can be determined according to actual conditions, such as 2, 4, 5, 10, etc. The washing room 310 of the present embodiment is provided with two.

[0058] Each washing room 310 of the present application is provided with a liquid inlet of washing liquid, which has the effect of enabling the washing liquid to be divided into multiple streams. When the material to be washed reaches each washing room 310, it contacts the cleaning washing liquid, thereby achieving multiple cleaning, and thus the material to be washed can be fully washed with a smaller amount of washing liquid.

[0059] The spiral continuous washing device of the present application is also provided with a feeding disperser 400 for dispersing the material to be washed and a liquid disperser 500 for dispersing the washing liquid, the feeding disperser 400 is assembled in the inside of the settling chamber 200, the liquid disperser 500 is assembled in the inside of the washing chamber 300, and each washing chamber 310 is provided with at least one liquid disperser 500. The feeding disperser 400 is the feeding port of the material to be washed in the vertical washing body. The liquid disperser 500 is the liquid inlet of the washing liquid in the vertical washing body. The material outlet 600 of the vertical washing body is located at the bottom of the washing chamber 300. The waste liquid outlet 700 of the vertical washing body is located at the side wall of the settling chamber 200.

[0060] The feeding disperser 400 and the liquid disperser 500 of the present application are both annular structures, and the surface of the annular structure is provided with a plurality of through holes; the annular structure surrounds the outer periphery of the stirrer 800 of the vertical washing body.

[0061] It should be noted that the feeding disperser 400 of the present application can uniformly transport the material to be washed to the settling chamber 200, and then uniformly enter the spiral channel 100. The liquid disperser 500 can make the washing liquid uniformly flow to the material to be washed, prevent the washing liquid from being excessive in some areas and insufficient in some areas, and obtain good fluidization conditions.

[0062] The stirrer 800 is provided with a stirring shaft, a plurality of middle stirring paddles 810 and a bottom stirring paddle 820, the middle stirring paddles 810 and the bottom stirring paddle 820 are fixedly assembled on the stirring shaft, the stirring shaft is fixedly assembled in the inside of the vertical washing body, and the stirring shaft is located in the stirring channel; there is at least one middle stirring paddle 810 in the range of each washing chamber 310, and the bottom stirring paddle 820 is located at the bottom of the washing chamber 300. The rotating direction of the middle stirring paddle 810 is opposite to the rotating direction of the spiral channel 100.

[0063] It should be noted that the middle stirring paddle 810 of the present application can generate a reverse power on the material to be washed, thereby reducing the downward flow speed of the material to be washed and increasing the contact time with the washing liquid. The bottom stirring paddle 820 can uniformly scatter the washed material on the bottom of the washing chamber 300, preventing the material from piling up and blocking the outlet 600.

[0064] The middle stirring paddle 810 of the present application can be a straight blade stirring paddle, an inclined blade stirring paddle, a propelling stirring paddle or a turbine stirring paddle, and the middle stirring paddle 810 is an upward stirring paddle. It should be noted that the type of the middle stirring paddle 810 can be determined according to the actual situation. The bottom stirring paddle 820 of the present application can be a straight blade stirring paddle, an inclined blade stirring paddle, a propelling stirring paddle or a turbine stirring paddle. It should be noted that the type of the bottom stirring paddle 820 can be determined according to the actual situation.

[0065] The outer diameter of the middle stirring paddle 810 is defined as D1, and the maximum inner diameter of the stirring channel is defined as D2, and there is 0.60D2≤D1≤0.95D2; the specific D1 of the embodiment is 0.80D2.

[0066] The outer diameter of the bottom stirring paddle 820 is defined as D3, and the maximum inner diameter of the washing cavity 300 is defined as D4, and there is 0.4D4≤D2≤0.95D4; the specific D2 of the embodiment is 0.5D4.

[0067] The diameter of the spiral channel 100 is defined as D5, and the pitch of the spiral channel 100 is defined as D6, and there is D5:D6=0.9-1.8, and the specific D5:D6 of the embodiment is 1. The opening rate of the annular structure is 15%-90%, and the specific opening rate is 30%.

[0068] The D1, D2, D3, D4, D5, D6 and the opening rate of the present application, the above-mentioned ratio and the specific value are determined according to the actual situation, as long as it is within the above-mentioned range, the washing effect of the spiral continuous washing equipment of the present application can be realized, and the residence time of the material can be adjusted by adjusting the diameter of the spiral channel 100 and the pitch of the spiral channel 100.

[0069] The present application has the following beneficial effects:

[0070] (1), the spiral channel 100 of the spiral continuous washing equipment increases the distance of the material to be washed in the washing equipment, so as to increase the contact time with the washing liquid and improve the washing effect;

[0071] (2), the spiral channel 100 of the spiral continuous washing equipment does not have dead angle, and the material does not accumulate inside, so as to improve the washing efficiency;

[0072] (3), the present application is an integrated vertical spiral continuous washing equipment, which can reduce the floor area of the equipment, compared with the horizontal washing equipment and the series washing equipment of the prior art, the spiral continuous washing equipment saves space by 50%;

[0073] (4), the spiral channel 100 of the present application is directly fixed in the interior of the vertical washing main body, the spiral channel 100 has low power consumption to the motor, and the stirrer 800 is located in the stirring channel of the spiral channel 100, so the cross-sectional area of the stirrer 800 is small, so as to further reduce the shaft power of the motor and reduce the power consumption;

[0074] (5), the washing liquid is divided into multiple strands and enters different washing cavities 300 respectively, forming a multi-stage washing effect, which can fully wash the material with a small amount of washing liquid, compared with the prior art, the spiral continuous washing equipment of the present application can save water by more than 30%;

[0075] (6), the washing material and washing liquid are respectively circular structure flow, play a uniform dispersion effect.

[0076] Embodiment 2

[0077] A spiral continuous washing equipment, other features are the same with embodiment 1, the difference is that:

[0078] The middle stirring paddle 810 of the embodiment is an upturned stirring paddle, which can generate a larger upward vortex of the washing material located in the middle of the washing cavity 300, thereby further increasing the residence time of the washing material.

[0079] The outer diameter of the middle stirring paddle 810 is defined as D1, and the maximum inner diameter of the stirring channel is defined as D2. When in the range of 0.70D2≤D1≤0.90D2, the stirring speed of the material is moderate, which ensures the residence time of the material and the discharge speed.

[0080] The outer diameter of the bottom stirring paddle 820 of the embodiment is the maximum inner diameter of the washing cavity 300, and when in the range of 0.5D4≤D2≤0.90D4, the material will not block the discharge port 600.

[0081] The diameter of the spiral channel 100 of the embodiment and the pitch of the spiral channel 100 are in the range of 1.0-1.5, and the speed of the material in this range is more moderate.

[0082] When the opening rate of the annular structure is 20%-85%, the flow rate of the material or the washing liquid can be better controlled, and when the opening rate is 80%, the washing effect is best verified by experiments.

[0083] Embodiment 3

[0084] A spiral continuous washing equipment, as shown in Figure 2 other features are the same with embodiment 1, the difference is that:

[0085] The washing chamber 310 of the embodiment is specifically provided with three, and the three washing chambers 310 are sequentially defined as a first-stage washing chamber 310, a second-stage washing chamber 310 and a third-stage washing chamber 310 from top to bottom. The middle stirring paddle 810 of the embodiment is an upturned stirring paddle. The bottom stirring paddle 820 is a straight-blade stirring paddle. The middle stirring paddle 810 is an upturned stirring paddle.

[0086] The D1 of the embodiment is 0.80D2, the D3 is 0.80D4, the diameter of the spiral channel 100 and the pitch of the spiral channel 100 are 1.2. The opening rate of the annular structure is 80%.

[0087] Embodiment 4

[0088] A spiral continuous washing device, other features are the same as example 1, the difference is that:

[0089] The washing chamber 310 of the embodiment is specifically provided with three, and the three washing chambers 310 are sequentially defined from top to bottom as a first-stage washing chamber 310, a second-stage washing chamber 310 and a third-stage washing chamber 310. The middle stirring paddle 810 of the embodiment is an upturned stirring paddle. The bottom stirring paddle 820 is a straight-blade stirring paddle. The middle stirring paddle 810 is an upturned stirring paddle.

[0090] In the embodiment, D1=0.60D2, D3=0.95D4, the diameter of the spiral channel 100 and the pitch of the spiral channel 100 are 0.9. The opening rate of the annular structure is 15%.

[0091] Example 5

[0092] A spiral continuous washing device, other features are the same as example 1, the difference is that:

[0093] The washing chamber 310 of the embodiment is specifically provided with three, and the three washing chambers 310 are sequentially defined from top to bottom as a first-stage washing chamber 310, a second-stage washing chamber 310 and a third-stage washing chamber 310. The middle stirring paddle 810 of the embodiment is an upturned stirring paddle. The bottom stirring paddle 820 is a straight-blade stirring paddle. The middle stirring paddle 810 is an upturned stirring paddle.

[0094] In the embodiment, D1=0.95D2, D3=0.40D4, the diameter of the spiral channel 100 and the pitch of the spiral channel 100 are 1.8. The opening rate of the annular structure is 90%.

[0095] Example 6

[0096] A solid washing method, using the spiral continuous washing device of example 3, specifically, when the washing liquid fills the spiral continuous washing device, the washing liquid is divided into multiple strands and enters each washing chamber 310 from the liquid inlet, the solid particle slurry to be washed enters from the feed inlet, the solid particle slurry to be washed flows through each washing chamber 310 along the spiral channel 100 from top to bottom, the washing liquid flows from bottom to top, the solid particle slurry to be washed and the washing liquid counterflow contact, and finally the washing liquid is discharged from the liquid outlet 700, and the washed solid particles are discharged from the discharge outlet 600.

[0097] The solid washing method, the solid particles flow from top to bottom along the spiral channel 100, the material does not accumulate inside, thereby improving the washing effect, the solid particles fall along the spiral channel 100 can increase the distance, so as to increase the contact time with the washing liquid, and improve the washing effect.

[0098] Example 7

[0099] A polyarylene sulfide washing method using the spiral continuous washing device of Example 3. Specifically, at room temperature and normal pressure, the washing liquid is divided into multiple strands and enters each washing chamber 310 from the liquid inlet. After the spiral continuous washing device is filled with the washing liquid, the slurry of the polyarylene sulfide to be washed is fed from the feed inlet, and the polyarylene sulfide to be washed flows along the spiral channel 100 from top to bottom through each washing chamber 310. The washing liquid flows from bottom to top, and the polyarylene sulfide to be washed and the washing liquid flow countercurrently. Finally, the washing liquid is discharged from the liquid outlet 700, and the washed polyarylene sulfide is discharged from the discharge outlet 600.

[0100] It should be noted that the contact time with the washing liquid is increased by using the spiral channel 100, so that the same washing effect as the prior art can be achieved at room temperature and normal pressure, thereby further reducing energy consumption.

[0101] The solid content of the slurry of the polyarylene sulfide to be washed is 10%-50%, and the washing liquid is an acetone solution with a concentration of 90%-100%. When the washing liquid is not a pure acetone solution, it is a mixed solution of acetone and water.

[0102] The polyarylene sulfide washing method, the solid particles flow from top to bottom along the spiral channel 100, and the material does not accumulate inside, thereby improving the washing efficiency. The solid particles falling along the spiral channel 100 can increase the distance, thereby increasing the contact time with the washing liquid and improving the washing effect. Finally, the NMP content of the final product of the present application is stably below 0.1%.

[0103] Example 8

[0104] A polyarylene sulfide washing method using the spiral continuous washing device of Example 3. Specifically, at room temperature and normal pressure, the washing liquid is divided into multiple strands and enters each washing chamber 310 from the liquid inlet. After the spiral continuous washing device is filled with the washing liquid, the slurry of the polyarylene sulfide to be washed is fed through the feed distribution ring and dispersed in the settling chamber. The slurry of the polyarylene sulfide to be washed and the washing liquid are continuously fed into the spiral continuous washing device, respectively. The polyarylene sulfide to be washed flows along the spiral channel 100 from top to bottom through each washing chamber 310. The washing liquid flows from bottom to top, and the polyarylene sulfide to be washed and the washing liquid flow countercurrently. The washing liquid countercurrently washes the slurry. Finally, the washing liquid is discharged from the liquid outlet 700, and the washed polyarylene sulfide is discharged from the discharge outlet 600. The solid content of the slurry of the polyarylene sulfide to be washed is 10%, the sodium chloride content is 5%, the NMP content is 5%, the PAS particle density is 1.4 g / cm 3 , and the particle size is 1000 μm. The washing liquid is an acetone aqueous solution with a concentration of 90%.

[0105] In this example, the feed amount of the slurry of the polyarylene sulfide to be washed is controlled to be 4500 kg / h, and the feed amount of the washing liquid is 3600 kg / h.

[0106] After washing, the output of polyarylene sulfide is 4500 kg / h, the sample of the effluent from the outlet 700 is detected, the salt content in the waste liquid is 3.84%, the salt content in the condensed slurry of the polyarylene sulfide outlet 600 is 0.08%, and the NMP content in the polyarylene sulfide is 0.06%.

[0107] Example 9

[0108] A polyarylene sulfide washing method is adopted, and the spiral continuous washing equipment of Example 3 is used. Specifically, at room temperature and normal pressure, the washing liquid is divided into multiple streams and enters each washing chamber 310 from the liquid inlet. After the spiral continuous washing equipment is filled with washing liquid, the slurry to be washed polyarylene sulfide is uniformly fed through the feed distribution ring and dispersed in the settling chamber. The slurry to be washed polyarylene sulfide and the washing liquid are continuously fed into the spiral continuous washing equipment, respectively. The slurry to be washed polyarylene sulfide flows along the spiral channel 100 from the bottom to the top through each washing chamber 310, and the washing liquid flows from the bottom to the top. The slurry to be washed polyarylene sulfide and the washing liquid are countercurrently contacted, and the washing liquid is countercurrently washed with the slurry. Finally, the washing liquid is discharged from the outlet 700, and the washed polyarylene sulfide is discharged from the outlet 600. The solid content of the slurry to be washed polyarylene sulfide is 20%, the sodium chloride content is 8%, the NMP content is 6%, and the PAS particle density is 1.4 g / cm 3 , and the particle size is 1000 μm. The washing liquid is an acetone solution with a concentration of 95%.

[0109] In this embodiment, the feeding amount of the slurry to be washed polyarylene sulfide is controlled to be 2000 kg / h, and the feeding amount of the washing liquid is 1600 kg / h.

[0110] After washing, the output of polyarylene sulfide is 2000 kg / h, the sample of the effluent from the outlet 700 is detected, the salt content in the waste liquid is 3.94%, the salt content in the condensed slurry of the polyarylene sulfide outlet 600 is 0.08%, and the NMP content in the polyarylene sulfide is 0.06%.

[0111] Example 10

[0112] A polyarylene sulfide washing method using the spiral continuous washing device of Example 3. Specifically, at room temperature and normal pressure, the washing liquid is divided into multiple strands and enters each washing chamber 310 from the liquid inlet. After the spiral continuous washing device is filled with washing liquid, the slurry of polyarylene sulfide to be washed is uniformly fed through the feed distribution ring and dispersed in the settling chamber. The slurry of polyarylene sulfide to be washed and the washing liquid are continuously fed into the spiral continuous washing device, respectively. The polyarylene sulfide to be washed flows from top to bottom through each washing chamber 310 along the spiral channel 100, and the washing liquid flows from bottom to top. The polyarylene sulfide to be washed and the washing liquid counterflow contact, and the washing liquid counterflow washes the slurry. Finally, the washing liquid is discharged from the liquid outlet 700, and the washed polyarylene sulfide is discharged from the discharge outlet 600. The solid content of the slurry of polyarylene sulfide to be washed is 20%, the sodium chloride content is 8%, the NMP content is 6%, and the PAS particle density is 1.4 g / cm 3 , and the particle size is 1000 μm. The washing liquid is an aqueous acetone solution with a concentration of 100%.

[0113] In this example, the feed amount of the slurry of polyarylene sulfide to be washed is controlled to be 2000 kg / h, and the feed amount of the washing liquid is 1600 kg / h.

[0114] After washing, the discharge amount of polyarylene sulfide is 2000 kg / h. The waste liquid in the liquid outlet 700 is detected, and the salt content is 3.85%. The slurry in the discharge outlet 600 of the polyarylene sulfide has a salt content of 0.08%, and the NMP content in the polyarylene sulfide is 0.07%.

[0115] Example 11

[0116] A polyarylene sulfide washing method using the spiral continuous washing device of Example 4. Specifically, at room temperature and normal pressure, the washing liquid is divided into multiple strands and enters each washing chamber 310 from the liquid inlet. After the spiral continuous washing device is filled with washing liquid, the slurry of polyarylene sulfide to be washed is uniformly fed through the feed distribution ring and dispersed in the settling chamber. The slurry of polyarylene sulfide to be washed and the washing liquid are continuously fed into the spiral continuous washing device, respectively. The polyarylene sulfide to be washed flows from top to bottom through each washing chamber 310 along the spiral channel 100, and the washing liquid flows from bottom to top. The polyarylene sulfide to be washed and the washing liquid counterflow contact, and the washing liquid counterflow washes the slurry. Finally, the washing liquid is discharged from the liquid outlet 700, and the washed polyarylene sulfide is discharged from the discharge outlet 600. The solid content of the slurry of polyarylene sulfide to be washed is 20%, the sodium chloride content is 8%, the NMP content is 6%, and the PAS particle density is 1.4 g / cm 3 , and the particle size is 1000 μm. The washing liquid is an aqueous acetone solution with a concentration of 95%.

[0117] In this embodiment, the feed rate of the polyarylene sulfide slurry to be washed is controlled at 2000 kg / h, and the feed rate of the washing liquid is controlled at 1600 kg / h.

[0118] After washing, the discharge rate of polyarylene sulfide is 2000 kg / h. The washing liquid sample from outlet 700 is tested and the salt content in the waste liquid is 3.78%. The salt content in the slurry from outlet 600 of polyarylene sulfide is 0.10%. The NMP content in polyarylene sulfide is 0.09%.

[0119] Example 12

[0120] A method for washing polyarylene sulfides (PNS) using the spiral continuous washing equipment described in Example 5. Specifically, at room temperature and atmospheric pressure, the washing liquid is divided into multiple streams and enters each washing chamber 310 through the inlet. After the spiral continuous washing equipment is filled with washing liquid, the PNS slurry to be washed is evenly fed through the feed distribution ring and dispersed in the settling chamber. The PNS slurry and washing liquid continuously enter the spiral continuous washing equipment. The PNS flows downwards through each washing chamber 310 along the spiral channel 100, while the washing liquid flows upwards. The PNS and washing liquid come into countercurrent contact, and the washing liquid washes the slurry countercurrently. Finally, the washing liquid is discharged from the outlet 700, and the washed PNS is discharged from the discharge outlet 600. The PNS slurry to be washed has a solid content of 20%, a sodium chloride content of 8%, an NMP content of 6%, and a PAS particle density of 1.4 g / cm³. 3 The particle size is 1000 μm. The washing solution is a 95% aqueous solution of acetone.

[0121] In this embodiment, the feed rate of the polyarylene sulfide slurry to be washed is controlled at 2000 kg / h, and the feed rate of the washing liquid is controlled at 1600 kg / h.

[0122] After washing, the discharge rate of polyarylene sulfide is 2000 kg / h. The washing liquid sample from outlet 700 is tested and the salt content in the waste liquid is 3.81%. The salt content in the slurry from outlet 600 of polyarylene sulfide is 0.09%. The NMP content in polyarylene sulfide is 0.07%.

[0123] Comparative Example 1

[0124] A method for washing polyarylene sulfides, using a tower-type solid-liquid countercurrent contact device disclosed in CN102781568A for cleaning.

[0125] Specifically, when the tower type solid-liquid countercurrent contact device is filled with the washing liquid at room temperature and normal pressure, the slurry of the polyarylene sulfide to be washed is fed and dispersed at the top of the tower, and the slurry of the polyarylene sulfide to be washed and the washing liquid are continuously fed into the device, respectively, to perform countercurrent washing on the slurry. The solid content of the slurry of the polyarylene sulfide to be washed is 50%, the sodium chloride content is 8%, the NMP content is 8%, the PAS particle density is 1.4 g / cm 3 , and the particle size is 1000 μm. The washing liquid is an aqueous acetone solution with a concentration of 90%.

[0126] The feeding amount of the slurry of the polyarylene sulfide to be washed in the comparative example is controlled to be 2000 kg / h, and the feeding amount of the washing liquid is controlled to be 1600 kg / h.

[0127] After washing, the discharging amount of the polyarylene sulfide is 2000 kg / h, the waste liquid in the outlet 700 of the washing liquid is detected, the salt content in the waste liquid is 1.24%, the salt content in the condensed slurry of the polyarylene sulfide in the outlet 600 of the polyarylene sulfide is 1.48%, and the NMP content in the polyarylene sulfide is 2.43%.

[0128] Comparative Example 2

[0129] A polyarylene sulfide washing method adopts a tower type solid-liquid countercurrent contact device for cleaning, which is disclosed in CN102781568A.

[0130] At normal pressure and 50°C, when the tower type solid-liquid countercurrent contact device is filled with the washing liquid, the slurry of the polyarylene sulfide to be washed is fed and dispersed at the top of the tower, and the slurry of the polyarylene sulfide to be washed and the washing liquid are continuously fed into the device, respectively, to perform countercurrent washing on the slurry. The solid content of the slurry of the polyarylene sulfide to be washed is 50%, the sodium chloride content is 8%, the NMP content is 8%, the PAS particle density is 1.4 g / cm 3 , and the particle size is 1000 μm. The washing liquid is an aqueous acetone solution with a concentration of 90%.

[0131] The feeding amount of the slurry of the polyarylene sulfide to be washed in the comparative example is controlled to be 2000 kg / h, and the feeding amount of the washing liquid is controlled to be 1600 kg / h.

[0132] After washing, the discharging amount of the polyarylene sulfide is 2000 kg / h, the waste liquid in the outlet 700 of the washing liquid is detected, the salt content in the waste liquid is 2.94%, the salt content in the condensed slurry of the polyarylene sulfide in the outlet 600 of the polyarylene sulfide is 0.34%, and the NMP content in the polyarylene sulfide is 0.52%.

[0133] Comparative Example 3

[0134] The spiral continuous washing equipment used in the present comparative example has the same features as example 1, except that the washing chamber 310 of the present example is specifically provided with three, and the three washing chambers 310 are sequentially defined as a first-stage washing chamber 310, a second-stage washing chamber 310 and a third-stage washing chamber 310 from top to bottom. The middle stirring paddle 810 of the present example is an upturned stirring paddle. The bottom stirring paddle 820 is a straight-blade stirring paddle. The middle stirring paddle 810 is an upturned stirring paddle. In the present example, D1 = 0.55D2, D3 = 0.30D4, the diameter of the spiral channel 100 and the pitch of the spiral channel 100 are 2.0. The opening rate of the annular structure is 10%.

[0135] The polyarylene sulfide washing method of the present comparative example uses the above-mentioned spiral continuous washing equipment. Specifically, under room temperature and normal pressure, the washing liquid is divided into multiple strands and enters each washing chamber 310 from the liquid inlet. After the spiral continuous washing equipment is filled with washing liquid, the slurry of the polyarylene sulfide to be washed is uniformly fed through the feed distribution ring and dispersed in the settling chamber. The slurry of the polyarylene sulfide to be washed and the washing liquid are continuously introduced into the spiral continuous washing equipment, respectively. The polyarylene sulfide to be washed flows through each washing chamber 310 along the spiral channel 100 from top to bottom, and the washing liquid flows from bottom to top. The polyarylene sulfide to be washed and the washing liquid counterflow contact, and the washing liquid counterflow washes the slurry. Finally, the washing liquid is discharged from the liquid outlet 700, and the washed polyarylene sulfide is discharged from the discharge outlet 600. The solid content of the slurry of the polyarylene sulfide to be washed is 20%, the sodium chloride content is 8%, the NMP content is 6%, the PAS particle density is 1.4 g / cm 3 , and the particle size is 1000 μm. The washing liquid is an aqueous acetone solution with a concentration of 90%.

[0136] The present comparative example controls the feed amount of the slurry of the polyarylene sulfide to be washed to be 2000 kg / h, and the feed amount of the washing liquid is 1600 kg / h.

[0137] After washing, the discharge amount of the polyarylene sulfide is 2000 kg / h. The waste liquid in the liquid outlet 700 is detected, and the salt content is 3.04%. The salt content of the slurry in the discharge outlet 600 of the polyarylene sulfide is 0.21%, and the NMP content in the polyarylene sulfide is 0.15%.

[0138] Finally, it should be noted that the above content is only used to illustrate the technical solutions of the present application, and is not a limitation on the protection scope of the present application. Simple modifications or equivalent replacements of the technical solutions of the present application made by those skilled in the art do not deviate from the essence and scope of the technical solutions of the present application.

Claims

1. A spiral continuous washing apparatus provided with a vertical washing main body, characterized by: At least one spiral channel for contacting the material to be washed with the washing liquid is arranged in the vertical washing body; The vertical washing body is provided with a settling chamber and a washing chamber, the settling chamber is arranged above the washing chamber, and the spiral channel is arranged in the washing chamber; The washing chamber is divided into at least two washing rooms from top to bottom, each of the washing rooms is provided with a liquid inlet of the washing liquid, and the spiral channel passes through all the washing rooms; A material disperser for dispersing the material to be washed and a liquid disperser for dispersing the washing liquid are arranged, the material disperser is arranged in the settling chamber, the liquid disperser is arranged in the washing chamber, and each of the washing rooms is provided with one liquid disperser; The material disperser is a material inlet of the vertical washing body; The liquid disperser is a liquid inlet of the vertical washing body; The material outlet of the vertical washing body is located at the bottom of the washing chamber; The liquid outlet of the vertical washing body is located at the side wall of the settling chamber; The material disperser and the liquid disperser are annular structures; The central axis of the spiral channel is provided with a hollow stirring channel for accommodating a stirrer; The stirrer is provided with a stirring shaft, a plurality of middle stirring paddles and a bottom stirring paddle, the middle stirring paddles and the bottom stirring paddle are fixedly arranged on the stirring shaft, the stirring shaft is fixed in the vertical washing body, and the stirring shaft is located in the stirring channel; There is at least one middle stirring paddle in the range of each of the washing rooms, and the bottom stirring paddle is located at the bottom of the washing chamber; The rotation direction of the middle stirring paddle is opposite to the rotation direction of the spiral channel; The outer diameter of the middle stirring paddle is defined as D1, the maximum inner diameter of the stirring channel is defined as D2, and there is 0.60D2≤D1≤0.95D2; The outer diameter of the bottom stirring paddle is defined as D3, the maximum inner diameter of the washing chamber is defined as D4, and there is 0.4D4≤D3≤0.95D4; The diameter of the spiral channel is defined as D5, and the pitch of the spiral channel is defined as D6, and there is D5:D6=0.9-1.8; The surface of the annular structure is provided with a plurality of through holes; the annular structure surrounds the outer periphery of the stirrer of the vertical washing body, and the opening rate of the annular structure is 15%-90%; The spiral channel guides the material to be washed to flow from top to bottom; The material to be washed is polyarylene sulfide slurry with a solid content of 10%-50%, and the washing liquid is 95%-100% acetone solution.

2. The spiral continuous washing apparatus according to claim 1, characterized by: The washing chamber is provided with three, and the three washing rooms are defined as a first-stage washing room, a second-stage washing room and a third-stage washing room from top to bottom.

3. The spiral continuous washing apparatus according to claim 1, characterized by: The bottom stirring paddle is a straight blade stirring paddle, an inclined blade stirring paddle, a propeller stirring paddle or a turbine stirring paddle; The middle stirring paddle is a straight blade stirring paddle, an inclined blade stirring paddle, a propeller stirring paddle or a turbine stirring paddle.

4. The spiral continuous washing apparatus according to claim 1, characterized by: The middle stirring paddle is an upward stirring paddle; The bottom of the settling chamber is funnel-shaped structure; The bottom of the washing chamber is funnel-shaped structure.

5. A polyarylene sulfide washing method characterized by: The spiral continuous washing equipment as claimed in any one of claims 1-4 is adopted, at room temperature and normal pressure, the washing liquid is divided into multiple strands and enters each washing chamber from the liquid inlet, the slurry of the polyarylene sulfide to be washed enters from the feed inlet, the polyarylene sulfide to be washed flows through each washing chamber from top to bottom along the spiral channel, the washing liquid flows from bottom to top, the polyarylene sulfide to be washed and the washing liquid are countercurrently contacted, finally the washing liquid is discharged from the liquid outlet, and the washed polyarylene sulfide is discharged from the discharge outlet; The solid content of the slurry of the polyarylene sulfide to be washed is 10%-50%; The washing liquid is an acetone solution with a concentration of 95%-100%.

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