CN109293854B - High-chroma impact-resistant polystyrene and preparation method and preparation device thereof - Google Patents
High-chroma impact-resistant polystyrene and preparation method and preparation device thereof Download PDFInfo
- Publication number
- CN109293854B CN109293854B CN201710615383.7A CN201710615383A CN109293854B CN 109293854 B CN109293854 B CN 109293854B CN 201710615383 A CN201710615383 A CN 201710615383A CN 109293854 B CN109293854 B CN 109293854B
- Authority
- CN
- China
- Prior art keywords
- unit
- liquid
- rubber
- impact
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/02—Recovery or working-up of waste materials of solvents, plasticisers or unreacted monomers
Abstract
The invention provides high-chroma impact-resistant polystyrene and a preparation method and a preparation device thereof, wherein the preparation device comprises a reaction unit, a devolatilization unit, a purification unit, a cooling unit, a liquid-liquid separation unit and a driving unit which are sequentially communicated, wherein the driving unit is respectively communicated with the reaction unit and a waste liquid collection unit; the liquid-liquid separation unit is communicated with the driving unit through a first pipeline, a cleaning liquid inlet and a cleaning liquid outlet are further formed in the first pipeline, the cleaning liquid inlet is formed in one end close to the liquid-liquid separation unit, and the cleaning liquid outlet is formed in one end close to the driving unit. The first pipe needs to be cleaned in the preparation process and the preparation raw materials in the reaction unit comprise linear structure rubber and/or a mixture of linear structure rubber and star-shaped rubber. The invention can not only obtain the impact-resistant polystyrene with high chroma, but also effectively control the chroma stability of the impact-resistant polystyrene.
Description
Technical Field
The invention relates to high-chroma impact-resistant polystyrene and a preparation method and a preparation device thereof, belonging to the technical field of synthetic resin.
Background
The high impact polystyrene is a product obtained by introducing rubber for improving the impact resistance of general polystyrene, the rubber generally used in industry is polybutadiene rubber and styrene-butadiene rubber, but Cl is introduced into the rubber product due to the addition of a coupling agent or a dispersing agent in the production process of any kind of rubber-，Cl-With Fe in the apparatus2+Formation of FeCl2。FeCl2Not only corrodes equipment, but also accumulates in a reaction system for a long time to form a wall built-up structure and fall off irregularly, so that the color of the high impact polystyrene product is influenced, and the appearance of the product is influenced.
Disclosure of Invention
The impact-resistant polystyrene product prepared by the method and the device has high Z-Y chromaticity, and the chromaticity of the impact-resistant polystyrene product can keep good stability in a six-month operation period.
The invention provides a preparation device of high-chroma impact-resistant polystyrene, which comprises a reaction unit, a devolatilization unit, a purification unit, a cooling unit, a liquid-liquid separation unit and a driving unit which are sequentially communicated, wherein the driving unit is respectively communicated with the reaction unit and a waste liquid collection unit;
the liquid-liquid separation unit is communicated with the driving unit through a first pipeline, a cleaning liquid inlet and a cleaning liquid outlet are further formed in the first pipeline, the cleaning liquid inlet is formed in one end close to the liquid-liquid separation unit, and the cleaning liquid outlet is formed in one end close to the driving unit.
In the device, the devolatilization unit comprises two outlets, wherein one outlet is a polymer outlet which can be directly communicated with the granulation unit to granulate the devolatilized polymer (i.e. the high-chroma impact-resistant polystyrene of the invention), the other outlet is a volatile component outlet, the volatile components are unreacted raw materials (rubber, styrene and ethylbenzene) and oligomerization products, the volatile component outlet is connected with the purification unit to separate oligomers in the volatile components, the residual unreacted raw materials can enter the cooling unit to be cooled, and then enter the liquid-liquid separation unit to stand, and then are driven by the driving unit to be input into the reaction unit again to be recycled to participate in the next polymerization reaction.
It is noted that the present invention further provides two openings on the first pipe connecting the liquid-liquid separation unit and the driving unit, that is, besides the openings at the two ends of the first pipe, two openings are further provided on the pipe body of the first pipe, one of the two openings is a cleaning liquid inlet disposed near the liquid-liquid separation unit, and the other opening is a cleaning liquid outlet disposed near the driving unit. The two openings are used for injecting cleaning liquid into the first pipeline to clean the first pipeline.
Specifically, the reactants in the reaction unit will introduce Cl into the system-As the volatile components pass through the purification unit, the cooling unit, the liquid-liquid separation unit and the Cl in sequence-Will interact with Fe in the device2+Formation of FeCl2And possibly some oligomers with small molecular weight which are not completely separated by the purification unit in the volatile component are also mixed with FeCl2Together in the system, the low molecular weight oligomers become sticky after being cooled by a cooling unit, especially with FeCl2The viscous substances enter the first pipeline from the liquid-liquid separation unit and adhere to the pipe wall of the first pipeline, and in order to prevent the viscous substances from being input into the reaction unit again by the driving unit to participate in new polymerization reaction so as to reduce the chroma of the polystyrene, the first pipeline needs to be cleaned, so that the cleaning liquid can carry the viscous substances out of the cleaning liquid outlet.
The reaction unit, the devolatilization unit, the purification unit, the cooling unit, the liquid-liquid separation unit and the driving unit in the device are not particularly limited by equipment, and can perform corresponding functions. For example, the reaction unit may be a reactor and the devolatilization unit may be a devolatilization reactor. The purification unit can be a purification tower, the cooling unit can be a water condenser, and the liquid-liquid separation unit can be a liquid receiving tank. The drive unit may be a drive pump and the waste liquid collection unit may be a collection tank.
The invention also provides a preparation method of the high-chroma impact-resistant polystyrene, which is carried out by utilizing the preparation device and comprises the following steps:
1) adding rubber, styrene and ethylbenzene into the reaction unit to carry out polymerization reaction to prepare a first product; wherein the rubber is linear structure rubber and/or a mixture of linear structure rubber and star-shaped rubber;
2) carrying out devolatilization treatment on the first product in the devolatilization unit, respectively collecting polymers and volatile components, and sequentially treating the volatile components through the purification unit, the cooling unit and the liquid-liquid separation unit to obtain a first collection; the polymer is high-chroma impact-resistant polystyrene;
3) conveying the first collection to the reaction unit through the driving unit for recycling;
wherein, before step 3), the method further comprises cleaning the first pipeline.
Specifically, the preparation of the impact polystyrene is mainly performed in the step 1), and the first product comprises the impact polystyrene obtained by the reaction and unreacted raw materials. In the preparation process, the invention limits the rubber in the raw materials, and particularly the rubber is a rubber with a linear structure and/or a mixture of the linear rubber and a rubber with a star-shaped structure. Because the content of chloride ions in the rubber with the star-shaped structure is 0.2-0.4 percent and is 1-4 times of that of the rubber with the linear structure, the proportion of the rubber with the star-shaped structure can be reduced on the premise of not influencing the quality of the impact-resistant polystyrene in order to avoid introducing excessive chloride ions. Generally, in the step 1), the rubber is 7-10 parts by weight, the styrene is 75-83 parts by weight, the ethylbenzene is 10-15 parts by weight, and the reaction temperature of the polymerization reaction is controlled to be 125-150 ℃ and the polymerization conversion rate is controlled to be 75-85%.
The devolatilization treatment of the first product in the step 2) mainly means to separate the polymer, the unreacted raw material and the oligomer produced in the polymerization reaction in the first product, wherein the unreacted raw material and the oligomer produced in the polymerization reaction are collectively referred to as volatile components. Generally, the devolatilization temperature of the devolatilization treatment can be controlled to be 220-240 ℃ and the devolatilization pressure can be controlled to be 0.1-8KPa, after the devolatilization is finished, the polymer can be separately collected and treated by granulation, etc., and the volatile component contains unreacted raw materials, so that the polymer can be collected and treated for recycling.
The volatile matter enters the purification unit firstly so as to enable the oligomer in the volatile matter to be discharged out of the purification unit, then the residual unreacted raw materials in the volatile matter enter the cooling unit for cooling, the cooling unit is generally in a water cooling mode, the cooling temperature is controlled to be room temperature, the cooling pressure is 0.1-0.13KPa, the unreacted raw materials enter the liquid-liquid separation unit after being cooled to the room temperature to generate a first collection, and then the first collection is input back to the reaction unit through the driving unit for repeated recycling.
It should be noted that before the first collection is input to the driving unit through the first pipeline, the first pipeline needs to be cleaned, which specifically includes: cleaning fluid is input into the first conduit through the cleaning fluid inlet and then discharged out of the first conduit through the cleaning fluid outlet. The present invention is not limited to the specific kind of the cleaning liquid as long as the viscous substance and the FeCl in the first tube can be cleaned2The cleaning agent can be flushed out, and normal-temperature and normal-pressure water can be used as the cleaning agent to save cost.
The present invention does not limit the specific time of the first pipe cleaning operation as long as the cleaning is performed before the first collected matter enters the first pipe. Before specific cleaning, an outlet of the liquid-liquid separation unit needs to be plugged, and after the cleaning is finished, the outlet of the liquid-liquid separation unit can be opened, so that the first collection enters the driving unit through the first pipeline and is input into the reaction unit by the driving unit.
In addition, in order to improve the working efficiency, the cleaning work for the first pipeline can be periodically performed, but the cleaning work for the first pipeline cannot be performed less than once per week, that is, the cleaning work for the first pipeline is performed at least once per week.
Since the rubber contains a certain amount of water, a part of water in the rubber is generated after the unreacted raw material is devolatilized and cooled, and thus the unreacted raw material is separated into layers of water and organic substances in the liquid-liquid separation unit, and FeCl is used as a material for the separation of organic substances from water2Will dissolve in water, so in order to improve the chromaticity of the product, the lower layer of water in the liquid-liquid separation unit should be discharged to the waste liquid collection unit in time. Specifically, the water discharge amount can be calculated according to the introduced amount of the rubber, and generally, in order to discharge the rubber completely, the water discharge amount can be 150% of the water content of the rubber.
The invention also provides high-chroma impact-resistant polystyrene which is prepared by the preparation method. The Z-Y chromaticity of the impact-resistant polystyrene can reach more than 12.
According to the invention, through selection of rubber types in reactants, regular flushing of pipelines and control of water discharge in the liquid-liquid separation unit, wall hanging formed by corrosion of equipment by chloride ions can be effectively reduced, the chromaticity of impact-resistant polystyrene is controlled, and the stability of chromaticity is maintained for a long time, so that the preparation method and the device are suitable for industrial production of high-chromaticity impact polystyrene.
Drawings
FIG. 1 is a view showing an apparatus for preparing high-chroma impact-resistant polystyrene according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages 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 accompanying drawings 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.
Example 1
The embodiment provides a device for preparing high-chroma impact-resistant polystyrene, fig. 1 is a device for preparing high-chroma impact-resistant polystyrene provided by the embodiment of the invention, please refer to fig. 1, the device comprises a reaction unit 1, a devolatilization unit 2, a purification unit 3, a cooling unit 4, a liquid-liquid separation unit 5 and a driving unit 6 which are sequentially communicated, and the driving unit 6 is respectively communicated with the reaction unit 1 and a waste liquid collection unit 7; specifically, the driving unit 6 is respectively communicated with the reaction unit 1 and the waste liquid collecting unit 7 through a tee joint, when liquid in the liquid-liquid separation unit 5 needs to be input into the reaction unit 1 through the driving unit 6, the tee joint can be rotated to enable the driving unit 6-the reaction unit 1 to be unblocked, and when liquid in the liquid-liquid separation unit 5 needs to be input into the waste liquid collecting unit 7 through the driving unit 6, the tee joint can be rotated to enable the driving unit 6-the waste liquid collecting unit 7 to be unblocked.
The liquid-liquid separation unit 5 is communicated with the driving unit 6 through a first pipeline 8, the first pipeline 8 is further provided with a cleaning liquid inlet 81 and a cleaning liquid outlet 82, the cleaning liquid inlet 81 is arranged at one end close to the liquid-liquid separation unit 5, and the cleaning liquid outlet 82 is arranged at one end close to the driving unit 6.
In this embodiment, the reaction unit 1 is a reactor, the devolatilization unit 2 is a devolatilization reactor, the purification unit 3 is a purification tower, the cooling unit 4 is a water condenser, the liquid-liquid separation unit 5 is a liquid receiving tank, the driving unit 6 is a liquid pump, and the waste liquid collection unit 7 is a common collection tank.
Example 2
This example used the production apparatus of example 1 to produce high-chroma impact-resistant polystyrene.
1. Stock preparation
7 parts of rubber, 83 parts of styrene and 10 parts of ethylbenzene, wherein the rubber is a mixture of rubber with a linear structure and rubber with a star structure according to a mass ratio of 1: 1. The volatile content (moisture) of the rubber with a linear structure is 0.5 percent, and the content of chloride ions is 0.08 percent; the volatile content (moisture) of the star-structured rubber was 0.6%, and the chloride ion content was 0.2%.
2. Reaction of
In the reaction unit 1, the rubber is dissolved in styrene and ethylbenzene, after the rubber is sufficiently dissolved, the temperature is raised to 128 ℃ for high-temperature polymerization, and when the polymerization conversion rate is 75%, the reaction slurry is fed into the devolatilization unit 2, and after high temperature of 220 ℃ and vacuum devolatilization of 8kpa, the polymer and the volatile matter (i.e., the produced oligomer and unreacted styrene monomer, ethylbenzene solvent and water in the rubber) are collected respectively.
3. Treatment of volatiles
The volatile is input into the purification unit 3, heavy components such as oligomers in the volatile are separated and discharged from the bottom of the purification unit 3, styrene, ethylbenzene, water and the like enter the cooling unit 4 from the top of the purification unit 3, are cooled by cooling water (the cooling water is at room temperature and the pressure is in a vacuum state of 0.13 ka), enter the liquid-liquid separation unit 5 for liquid level stratification, and are input into the reaction unit through the driving unit 6 for recycling. Wherein the first pipe 8 is flushed with water once every 3 days.
The preparation of the impact-resistant polystyrene was repeated according to the above steps 1 to 3, and the Z-Y chromaticity of the impact-resistant polystyrene prepared in this example was monitored for 7 days, and the results are shown in Table 1.
Example 3
This example used the production apparatus of example 1 to produce high-chroma impact-resistant polystyrene.
1. Stock preparation
8 parts of rubber, 80 parts of styrene and 12 parts of ethylbenzene, wherein the rubber is a mixture of rubber with a linear structure and rubber with a star structure according to a mass ratio of 2: 3. The volatile content (moisture) of the rubber with a linear structure is 0.7 percent, and the content of chloride ions is 0.1 percent; the volatile content (moisture) of the star-structured rubber was 0.8%, and the chloride ion content was 0.25%.
2. Reaction of
In the reaction unit 1, the rubber was dissolved in styrene and ethylbenzene, and after the rubber was sufficiently dissolved, the temperature was raised to 130 ℃ to perform high-temperature polymerization, and when the polymerization conversion rate was 78%, the reaction slurry was fed into the devolatilization unit 2, and after high-temperature devolatilization at 225 ℃ and vacuum devolatilization at 6kpa, the polymer and the volatile matter (i.e., the produced oligomer and unreacted styrene monomer, ethylbenzene solvent, and water in the rubber) were collected, respectively.
3. Treatment of volatiles
The volatile is input into the purification unit 3, heavy components such as oligomers in the volatile are separated and discharged from the bottom of the purification unit 3, styrene, ethylbenzene, water and the like enter the cooling unit 4 from the top of the purification unit 3, are cooled by cooling water (the cooling water is at room temperature and the pressure is in a vacuum state of 0.13 ka), enter the liquid-liquid separation unit 5 for liquid level stratification, and are input into the reaction unit through the driving unit 6 for recycling. Wherein the first pipe 8 is flushed with water once every 4 days.
The preparation of the impact-resistant polystyrene was repeated according to the above steps 1 to 3, and the Z-Y chromaticity of the impact-resistant polystyrene prepared in this example was monitored for 7 days, and the results are shown in Table 1.
Example 4
This example used the production apparatus of example 1 to produce high-chroma impact-resistant polystyrene.
1. Stock preparation
7.5 parts of rubber, 80 parts of styrene and 12.5 parts of ethylbenzene, wherein the rubber is a mixture of rubber with a linear structure and rubber with a star structure according to the mass ratio of 1: 1. The volatile content (moisture) of the rubber with a linear structure is 0.62 percent, and the content of chloride ions is 0.1 percent; the volatile content (moisture) of the star-structured rubber was 0.60%, and the chloride ion content was 0.2%.
2. Reaction of
In the reaction unit 1, the rubber is dissolved in styrene and ethylbenzene, after the rubber is sufficiently dissolved, the temperature is raised to 131 ℃ for high-temperature polymerization, and when the polymerization conversion rate is 80%, the reaction slurry is fed into the devolatilization unit 2, and after the high temperature of 230 ℃ and the vacuum devolatilization of 0.3kpa are performed, the polymer and the volatile matter (i.e., the produced oligomer and unreacted styrene monomer, ethylbenzene solvent and water in the rubber) are collected respectively.
3. Treatment of volatiles
Inputting the volatile into a purification unit 3, separating heavy components such as oligomers in the volatile from the bottom of the purification unit 3, discharging the heavy components such as styrene, ethylbenzene, water and the like from the top of the purification unit 3 into a cooling unit 4, cooling by cooling water (the cooling water is at room temperature and the pressure is in a vacuum state of 0.13 ka), introducing into a liquid-liquid separation unit 5 for liquid level stratification, and discharging water in the liquid-liquid separation unit 5 into a waste liquid collection unit 7, wherein the discharge amount is 150% of the rubber water content. The residual organic phase is input into the reaction unit through the driving unit 6 for recycling. Wherein the first pipe 8 is flushed with water once every 5 days.
The preparation of the impact-resistant polystyrene was repeated according to the above steps 1 to 3, and the Z-Y chromaticity of the impact-resistant polystyrene prepared in this example was monitored for 7 days, and the results are shown in Table 1.
Example 5
This example used the production apparatus of example 1 to produce high-chroma impact-resistant polystyrene.
1. Stock preparation
10 parts of rubber, 75 parts of styrene and 15 parts of ethylbenzene, wherein the rubber is a mixture of rubber with a linear structure and rubber with a star structure according to a mass ratio of 1: 1. The volatile content (moisture) of the rubber with a linear structure is 0.78 percent, and the content of chloride ions is 0.15 percent; the volatile content (moisture) of the star-structured rubber was 0.72%, and the chloride ion content was 0.3%.
2. Reaction of
In the reaction unit 1, the rubber was dissolved in styrene and ethylbenzene, and after the rubber was sufficiently dissolved, the temperature was raised to 140 ℃ to perform high-temperature polymerization, and when the polymerization conversion rate was 83%, the reaction slurry was fed into the devolatilization unit 2, and after the high temperature of 235 ℃ and the vacuum devolatilization of 0.15kpa, the polymer and the volatile matter (i.e., the produced oligomer and unreacted styrene monomer, ethylbenzene solvent, and water in the rubber) were collected, respectively.
3. Treatment of volatiles
Inputting the volatile into a purification unit 3, separating heavy components such as oligomers in the volatile from the bottom of the purification unit 3, discharging the heavy components such as styrene, ethylbenzene, water and the like from the top of the purification unit 3 into a cooling unit 4, cooling by cooling water (the cooling water is at room temperature and the pressure is in a vacuum state of 0.13 ka), introducing into a liquid-liquid separation unit 5 for liquid level stratification, and discharging water in the liquid-liquid separation unit 5 into a waste liquid collection unit 7, wherein the discharge amount is 150% of the rubber water content. The residual organic phase is input into the reaction unit through the driving unit 6 for recycling. Wherein the first pipe 8 is flushed with water once every 7 days.
The preparation of the impact-resistant polystyrene was repeated according to the above steps 1 to 3, and the Z-Y chromaticity of the impact-resistant polystyrene prepared in this example was monitored for 7 days, and the results are shown in Table 1.
Comparative example 1
This comparative example used the production apparatus in example 1 to produce impact-resistant polystyrene.
1. Stock preparation
10 parts of star-structured rubber, 75 parts of styrene and 15 parts of ethylbenzene, wherein the volatile component (moisture) of the star-structured rubber is 0.78%, and the content of chloride ions is 0.4%.
2. Reaction of
In the reaction unit 1, the rubber was dissolved in styrene and ethylbenzene, and after the rubber was sufficiently dissolved, the temperature was raised to 145 ℃ to perform high-temperature polymerization, and when the polymerization conversion rate was 85%, the reaction slurry was fed into the devolatilization unit 2, and after high-temperature removal at 238 ℃ and vacuum devolatilization at 0.1kpa, the polymer and the volatile matter (i.e., the produced oligomer and unreacted styrene monomer, ethylbenzene solvent, and water in the rubber) were collected, respectively.
3. Treatment of volatiles
Inputting the volatile into a purification unit 3, separating heavy components such as oligomers in the volatile from the bottom of the purification unit 3, discharging the heavy components such as styrene, ethylbenzene, water and the like from the top of the purification unit 3 into a cooling unit 4, cooling by cooling water (the cooling water is at room temperature and the pressure is in a vacuum state of 0.13 ka), introducing into a liquid-liquid separation unit 5 for liquid level stratification, and discharging water in the liquid-liquid separation unit 5 into a waste liquid collection unit 7, wherein the discharge amount is 150% of the rubber water content. The residual organic phase is input into the reaction unit through the driving unit 6 for recycling. The first pipe 8 is not cleaned.
The impact polystyrene was prepared by repeating the above steps 1 to 3, and the Z-Y chromaticity test was carried out on the impact polystyrene prepared in this comparative example for 7 days, and the results are shown in Table 1.
Comparative example 2
This comparative example used the production apparatus of example 1 to produce high-chroma impact polystyrene.
1. Stock preparation
8 parts of rubber, 79.5 parts of styrene and 12.5 parts of ethylbenzene, wherein the rubber is a mixture of rubber with a linear structure and rubber with a star structure according to the mass ratio of 1: 1. The volatile content (moisture) of the rubber with a linear structure is 0.67 percent, and the content of chloride ions is 0.1 percent; the volatile content (moisture) of the star-structured rubber was 0.72%, and the chloride ion content was 0.4%.
2. Reaction of
In the reaction unit 1, the rubber was dissolved in styrene and ethylbenzene, and after the rubber was sufficiently dissolved, the temperature was raised to 140 ℃ to perform high-temperature polymerization, and when the polymerization conversion rate was 82%, the reaction slurry was fed into the devolatilization unit 2 and subjected to high-temperature 225 ℃ and vacuum devolatilization at 0.15kpa, and then the polymer and the volatile matter (i.e., the produced oligomer and unreacted styrene monomer, ethylbenzene solvent, and water in the rubber) were collected, respectively.
3. Treatment of volatiles
Inputting the volatile into a purification unit 3, separating heavy components such as oligomers in the volatile from the bottom of the purification unit 3, discharging the heavy components such as styrene, ethylbenzene, water and the like from the top of the purification unit 3 into a cooling unit 4, cooling by cooling water (the cooling water is at room temperature and the pressure is in a vacuum state of 0.13 ka), introducing into a liquid-liquid separation unit 5 for liquid level stratification, and discharging water in the liquid-liquid separation unit 5 into a waste liquid collection unit 7, wherein the discharge amount is 150% of the rubber water content. The residual organic phase is input into the reaction unit through the driving unit 6 for recycling. The first pipe 8 is not cleaned.
The impact polystyrene was prepared by repeating the above steps 1 to 3, and the Z-Y chromaticity test was carried out on the impact polystyrene prepared in this comparative example for 7 days, and the results are shown in Table 1.
Comparative example 3
This comparative example used the production apparatus of example 1 to produce high-chroma impact-resistant polystyrene.
1. Stock preparation
7.8 parts of rubber, 79.7 parts of styrene and 12.5 parts of ethylbenzene, wherein the rubber is a mixture of rubber with a linear structure and rubber with a star structure according to the mass ratio of 1: 1. The volatile content (moisture) of the rubber with a linear structure is 0.62 percent, and the content of chloride ions is 0.1 percent; the volatile content (moisture) of the star-structured rubber was 0.68%, and the chloride ion content was 0.4%.
2. Reaction of
In the reaction unit 1, the rubber was dissolved in styrene and ethylbenzene, and after the rubber was sufficiently dissolved, the temperature was raised to 150 ℃ to perform high-temperature polymerization, and when the polymerization conversion rate was 83%, the reaction slurry was fed into the devolatilization unit 2, and after high-temperature and 0.4kpa vacuum devolatilization, the polymer and the volatile matter (i.e., the produced oligomer and unreacted styrene monomer, ethylbenzene solvent, and water in the rubber) were collected, respectively.
3. Treatment of volatiles
Inputting the volatile into a purification unit 3, separating heavy components such as oligomers in the volatile from the bottom of the purification unit 3, discharging the heavy components such as styrene, ethylbenzene, water and the like from the top of the purification unit 3 into a cooling unit 4, cooling by cooling water (the cooling water is at room temperature and the pressure is in a vacuum state of 0.13 ka), introducing into a liquid-liquid separation unit 5 for liquid level stratification, and discharging water in the liquid-liquid separation unit 5 into a waste liquid collection unit 7, wherein the discharge amount is 150% of the rubber water content. The residual organic phase is input into the reaction unit through the driving unit 6 for recycling. The first pipe 8 is not cleaned.
The impact-resistant polystyrene was prepared by repeating the above steps 1 to 3, and the Z-Y chromaticity test was carried out on the impact-resistant polystyrene prepared in the comparative example within 7 days, and the results are shown in table 1.
TABLE 1Z-Y chromaticity fluctuation ranges of impact-resistant polystyrenes prepared in examples and comparative examples
From the data in table 1, it can be seen that: the preparation method is suitable for stably producing high-chroma impact-resistant polystyrene.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. The preparation method of the high-chroma impact-resistant polystyrene is characterized by comprising the following steps of:
the preparation device comprises a reaction unit, a devolatilization unit, a purification unit, a cooling unit, a liquid-liquid separation unit and a driving unit which are sequentially communicated, wherein the driving unit is respectively communicated with the reaction unit and the waste liquid collection unit;
the liquid-liquid separation unit is communicated with the driving unit through a first pipeline, a cleaning liquid inlet and a cleaning liquid outlet are formed in the first pipeline, the cleaning liquid inlet is formed in one end close to the liquid-liquid separation unit, and the cleaning liquid outlet is formed in one end close to the driving unit;
the method comprises the following steps:
1) adding rubber, styrene and ethylbenzene into the reaction unit to carry out polymerization reaction to prepare a first product; wherein the rubber is linear structure rubber and/or a mixture of linear structure rubber and star-shaped rubber;
2) carrying out devolatilization treatment on the first product in the devolatilization unit, respectively collecting polymers and volatile components, and sequentially treating the volatile components through the purification unit, the cooling unit and the liquid-liquid separation unit to obtain a first collection; the polymer is high-chroma impact-resistant polystyrene;
3) conveying the first collection to the reaction unit through the driving unit for recycling;
before the step 3), cleaning the first pipeline;
the cleaning of the first pipeline specifically comprises: inputting a cleaning liquid into the first pipeline through the cleaning liquid inlet, and then discharging the cleaning liquid out of the first pipeline through the cleaning liquid outlet;
the frequency of cleaning the first pipeline is as follows: at least once per week;
before step 3), the method further comprises the following steps: and discharging the water in the first collection to the waste liquid collection unit through the driving unit, wherein the water is discharged according to 150% of the water content of the rubber.
2. The method for preparing high-chroma impact-resistant polystyrene as claimed in claim 1, wherein in the step 1), the rubber is 7 to 10 parts by weight, the styrene is 75 to 83 parts by weight, and the ethylbenzene is 10 to 15 parts by weight.
3. The method as claimed in claim 2, wherein the reaction temperature of the polymerization reaction in step 1) is controlled to be 125-150 ℃ and the polymerization conversion rate is controlled to be 75-85%.
4. The method as claimed in claim 3, wherein the devolatilization temperature of the devolatilization process is controlled to be 220-240 ℃ and the devolatilization pressure is controlled to be 0.1-8KPa in step 2).
5. The method for preparing high-chroma impact-resistant polystyrene as claimed in claim 4, wherein in the step 2), the cooling temperature of the cooling unit is controlled to be room temperature, and the cooling pressure is controlled to be 0.1 to 0.13 KPa.
6. A high-chroma impact-resistant polystyrene, characterized by being produced by the production method according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710615383.7A CN109293854B (en) | 2017-07-25 | 2017-07-25 | High-chroma impact-resistant polystyrene and preparation method and preparation device thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710615383.7A CN109293854B (en) | 2017-07-25 | 2017-07-25 | High-chroma impact-resistant polystyrene and preparation method and preparation device thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109293854A CN109293854A (en) | 2019-02-01 |
| CN109293854B true CN109293854B (en) | 2021-01-29 |
Family
ID=65167990
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710615383.7A Active CN109293854B (en) | 2017-07-25 | 2017-07-25 | High-chroma impact-resistant polystyrene and preparation method and preparation device thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109293854B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5714609A (en) * | 1980-06-30 | 1982-01-25 | Toyo Soda Mfg Co Ltd | Prevention of the formation and deposition of polymer scale |
| CN87105196A (en) * | 1986-07-25 | 1988-05-04 | 柯斯登技术公司 | The continuous production method of high impact polystyrene |
| CN1328068A (en) * | 2000-06-12 | 2001-12-26 | 吉林华标化学工业有限责任公司 | Process for preparing high-property high-impactness polystyrene |
| CN101341174A (en) * | 2005-12-21 | 2009-01-07 | 雅宝公司 | Brominated anionic styrenic polymers and their preparation |
| CN103773627A (en) * | 2012-10-23 | 2014-05-07 | 中国石油化工股份有限公司 | Solution for cleaning polylactic acid polymerization reaction device and cleaning method |
-
2017
- 2017-07-25 CN CN201710615383.7A patent/CN109293854B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5714609A (en) * | 1980-06-30 | 1982-01-25 | Toyo Soda Mfg Co Ltd | Prevention of the formation and deposition of polymer scale |
| CN87105196A (en) * | 1986-07-25 | 1988-05-04 | 柯斯登技术公司 | The continuous production method of high impact polystyrene |
| CN1328068A (en) * | 2000-06-12 | 2001-12-26 | 吉林华标化学工业有限责任公司 | Process for preparing high-property high-impactness polystyrene |
| CN101341174A (en) * | 2005-12-21 | 2009-01-07 | 雅宝公司 | Brominated anionic styrenic polymers and their preparation |
| CN103773627A (en) * | 2012-10-23 | 2014-05-07 | 中国石油化工股份有限公司 | Solution for cleaning polylactic acid polymerization reaction device and cleaning method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109293854A (en) | 2019-02-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101056922B (en) | Method for purifying a solution containing a plastic material | |
| US11692087B2 (en) | Process for producing monovinylaromatic polymer incorporating post-consumer recycled polystyrene, monovinylaromatic polymer incorporating post-consumer recycled polystyrene and articles produced thereof | |
| CN110563870B (en) | Industrial production method of synthetic rubber and industrial device for implementing method | |
| CN109293854B (en) | High-chroma impact-resistant polystyrene and preparation method and preparation device thereof | |
| CN105693899B (en) | The device and its production method of micro- outstanding newborn method production PVC paste resin | |
| CN100358815C (en) | Process and equipment for treating PVC centrifugal mother liquor | |
| CN111233612B (en) | Efficient polymerization inhibitor for extracting and separating carbon five by DMF (dimethyl formamide) method and application method thereof | |
| CN104368175A (en) | Dynamic gas-liquid separator | |
| CN103755509B (en) | Styrene-butadiene rubber styrene recycling process and device | |
| CN110548331A (en) | method and device for separating polymer in slurry method polyethylene production process | |
| CN113736135B (en) | Method and device for recycling chlorine-containing waste plastics and heavy oil blending component | |
| CN113912754A (en) | Technical combination method for removing VOCs and odor from polyolefin resin | |
| JP6740220B2 (en) | Method for producing methyl methacrylate with reduced pollution | |
| CN114272878A (en) | Devolatilization and feeding two-in-one device, solution polymerization device and polymerization method | |
| CN210506173U (en) | Light component extraction device of polypropylene process reactor | |
| EP3104949B1 (en) | Divalent ion removal from monoethylene glycol (meg) feed streams | |
| KR20130108809A (en) | Method of preparing lignin-polyester resin mixed powder and lignin-polyester resin mixed powder by the same | |
| CN106540472A (en) | The condensing method of rubber polymer condensing field and coacervation device and rubber polymer solution | |
| CN214020695U (en) | Polycarbonate reactor washs material returned device | |
| CN206838031U (en) | A kind of system of acetylene and formaldehyde deep reaction | |
| CN205616830U (en) | Hang device of newborn method production PVC paste resin a little | |
| WO2018105851A1 (en) | System for reclaiming sewage/wastewater for reuse | |
| CN203668267U (en) | Device for recovering styrene in styrene butadiene rubber | |
| CN219771928U (en) | Styrene wastewater treatment system | |
| CN113698716B (en) | Composite material for tubular membrane and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |