CN111151037A - Method and system for hydrocyclone separation of ultra high molecular weight polyethylene slurry - Google Patents
Method and system for hydrocyclone separation of ultra high molecular weight polyethylene slurry Download PDFInfo
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- CN111151037A CN111151037A CN202010043502.8A CN202010043502A CN111151037A CN 111151037 A CN111151037 A CN 111151037A CN 202010043502 A CN202010043502 A CN 202010043502A CN 111151037 A CN111151037 A CN 111151037A
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- B01D21/26—Separation of sediment aided by centrifugal force or centripetal force
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Abstract
The invention discloses a method and a system for separating ultra-high molecular weight polyethylene slurry by hydrocyclone, and the method comprises a method for separating ultra-high molecular weight polyethylene slurry by hydrocyclone. The system consists of a hydrocyclone, a drier, a washing tower and a condenser, and the devices are connected in combination through pipelines. The method and the system for separating the ultra-high molecular weight polyethylene slurry by the hydrocyclone adopt the hydrocyclone to carry out solid-liquid separation on the polyethylene slurry, so that the bulk materials are settled to the bottom of the hydrocyclone and are sent to a subsequent dryer together with the polyethylene wet cake, and the phenomenon that the centrifuge is stopped due to the blockage of the bulk materials is avoided; the method and the system for separating the slurry of the ultra-high molecular weight polyethylene by the hydrocyclone are used in the industrial production of the ultra-high molecular weight UHMWPE polyethylene, the operation period of the ultra-high molecular weight UHMWPE polyethylene device is prolonged from 3-5 months of a centrifugal machine in the prior art to 18-20 months of the hydrocyclone, and the method and the system have good popularization and application values.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method and a system for separating ultra-high molecular polyethylene slurry by hydrocyclone.
Background
The ultra-high molecular weight UHMWPE polyethylene is a polyethylene resin with a molecular weight of 150-800 ten thousand. Because the UHMWPE polyethylene has larger molecular weight, the UHMWPE polyethylene has the excellent performances of impact resistance, abrasion resistance, low temperature resistance, corrosion resistance, self lubrication and the like, and has wide application. In addition, the UHMWPE can also be applied to two important application fields of super-strong polyethylene fibers, lithium battery diaphragms and the like. In the process of preparing UHMWPE polyethylene, polyethylene reaction slurry containing 50-80 wt% of hexane is continuously added to a high-speed rotating horizontal centrifuge through a slurry conveying pump, and after centrifugal separation, polyethylene wet cake and hexane mother liquor are separated. And conveying the polyethylene wet cake containing 15-45 wt% of hexane to a dryer, drying by nitrogen to obtain polyethylene dry powder, and conveying the polyethylene dry powder to an extrusion granulation unit. And (4) after gas stripping, sending the hexane mother liquor to a solvent recovery section for recycling. Thereby carrying out the solid-liquid separation operation of the UHMWPE solid particles and the hexane liquid solvent.
In the prior art, the invention patent application No. 201510142391.5 discloses a method for producing polyethylene by tank type slurry, application and the produced polyethylene, firstly, ethylene raw material, titanium tetrachloride serving as a main catalyst, triethyl aluminum serving as a cocatalyst, hexane serving as a solvent, hydrogen, propylene or butene-1 and other materials are added into a reactor to generate polymerization reaction; secondly, conveying the polymerization slurry to a powder dryer for flash evaporation and carrying out filter pressing on the polymerization slurry to realize liquid-solid separation; then, drying the material under reduced pressure, and introducing nitrogen to remove hexane in the powder; finally, removing gel from the polyethylene powder through a vibrating screen, and then flowing into a powder bin for storage; the ethylene feed rate of the invention is 100kg/h, corresponding to a polyethylene production capacity of 800 tons/year. The invention patent application No. 201811056162.1 discloses a composite material of ultra-high molecular weight polyethylene film and a preparation method thereof, which comprises the steps of firstly modifying ultra-high molecular weight polyethylene, secondly granulating through a double-screw extruder, then extruding into sheets through a single-screw extruder, then calendering through a multi-roll calender, and further winding into the film. Invention patent application No. 201910213170.0, a process for preparing an ultra high molecular weight polyethylene composition, discloses the preparation of high molecular weight polyethylene without hydrogenation in a first stage polymerization process; in the second stage of polymerization, a small amount of hydrogen is added to prepare low molecular weight polyethylene; thereby eliminating the need for dehydrogenation after the first stage polymerization is completed in the production of ultra high molecular weight polyethylene.
However, the above prior patent application No. 201510142391.5 only describes a process for producing polyethylene by polymerization, liquid-solid separation, drying under reduced pressure, and vibration separation, wherein the liquid-solid separation of the polymerization slurry adopts unit operations such as flash evaporation, filter pressing, etc., and the production capacity is only 800 tons/year, which is not a commercial large-scale industrial production technology. The invention patent application No. 201811056162.1 and the invention patent application No. 201910213170.0 disclose only methods for preparing ultra-high molecular weight polyethylene films or ultra-high molecular weight polyethylene compositions, and do not relate to a slurry liquid-solid separation process of polyethylene containing hexane solvent.
In the prior art, in the technical process of producing common polyethylene products, the polyethylene slurry is separated in a centrifugal mode, so that the problem is solved, the separation efficiency is high, and the solid-liquid separation is sufficient. However, in the production process of the UHMWPE polyethylene with the ultrahigh molecular weight, the residence time of part of the catalyst and the polyethylene in the polymerization reactor in the reaction kettle can reach several times of the average residence time, and the possibility of generating blocky materials and large-particle materials with the particle size of more than 1.2 mm is gradually increased along with the increase of the residence time in the reaction kettle. No matter how the catalyst is improved, more or less 1-3 wt% of blocky materials and large-particle materials with the particle size larger than 1.2 mm are generated. And the outer brim of the centrifuge has a gap of 2 mm, so that the gap of the centrifuge is easily blocked by massive materials and large-particle materials in slurry polyethylene, thereby causing the shutdown of the centrifuge. Generally, after a centrifugal machine of an ultrahigh molecular weight UHMWPE device in the prior art runs for 3-5 months, the centrifugal machine has to be stopped for maintenance, and impurities accumulated in gaps of the centrifugal machine are removed.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method and a system for separating ultra-high molecular weight polyethylene slurry by using a hydrocyclone, which are used for carrying out solid-liquid separation on ultra-high molecular weight UHMWPE device slurry, meet the requirements of solid-liquid separation and reduce the shutdown times of a production device, and can be applied to large-scale commercial industrial production for preparing ultra-high molecular weight UHMWPE.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the invention provides a method for hydrocyclone separation of ultra-high molecular weight polyethylene slurry, which is applied to a large-scale commercial ultra-high molecular weight UHMWPE polyethylene industrial production device and is characterized by comprising the following steps:
s1, feeding the hexane-containing ultrahigh molecular weight UHMWPE polyethylene reaction slurry from the upstream process into a hydrocyclone; in the hydrocyclone separator, polyethylene reaction slurry containing hexane enters the hydrocyclone separator from a feeding pipe along a tangent line to form a rotational flow, the outer layer is a descending rotational flow, and polyethylene particles descend to form polyethylene wet cakes containing hexane; the inner layer is ascending rotational flow, and the hexane liquid ascends to form a hexane solvent without polyethylene particles;
s2, overflowing the hexane solvent separated by the hydrocyclone from the upper part of the dryer, and simultaneously falling the hexane-containing polyethylene wet cake separated by the hydrocyclone from the lower part of the dryer through a head difference into the dryer for further drying;
s3, conveying the dried polyethylene powder obtained in the dryer to a subsequent granulation process, and allowing the nitrogen-containing hexane mixed gas separated from the dryer to enter a washing tower, refining and purifying the nitrogen-containing hexane mixed gas and then allowing the nitrogen-containing hexane mixed gas to flow out from the top of the washing tower; the hexane at the top of the washing tower is combined with the hexane separated by the hydrocyclone into hexane which is sent to the hexane recovery process;
and S4, combining dry nitrogen from the outside with the circulating material flow, feeding the combined dry nitrogen and the circulating material flow into a dryer, drying the polyethylene wet cake, feeding the nitrogen-containing hexane mixed gas discharged from the dryer into a washing tower, feeding the material flow at the top of the washing tower into a condenser, refluxing hexane condensed in the condenser into the washing tower, combining one part of noncondensable nitrogen with the dry nitrogen, returning the combined dry nitrogen to the dryer again, and discharging the other part of material flow to the outside.
Further, in step S1, the density of polyethylene particle solid in the polyethylene reaction slurry from the upstream process is 870-990 kg/cm3, the density of hexane solvent liquid is 500-850 kg/m3, the particle size of the UHMWPE polyethylene solid particle is 10-1500 microns, the average particle size of the particle is 100-700 microns, the hexane content is 50-80 wt%, and the content of polyethylene wet cake hexane separated by a hydrocyclone is 15-45 wt%;
further, in step S3, the content of hexane in the dried polyethylene powder flowing out of the dryer is 0.1-2.0 wt%;
further, the production capacity of the ultrahigh molecular weight UHMWPE polyethylene production device is 1.0-15.0 ten thousand tons per year of large-scale commercial industrial device.
Further, in the steps S1-S2, the operating pressure of the hydrocyclone is 0.01-0.06 MPaG, and the operating temperature is 20-100 ℃.
Further preferably, in the steps S1-S2, the operating pressure of the hydrocyclone is 0.02-0.05 MPaG, and the operating temperature is 30-90 ℃.
Further, in the steps S3-S4, the operation pressure of the dryer is 0.002-0.042 MPaG, and the operation temperature is 20-120 ℃; the mechanical structure of the dryer is one of a disc dryer, a fluidized bed dryer or a steam steaming tank.
Further preferably, in the steps S3-S4, the dryer is preferably operated at a pressure of 0.007-0.037 MPaG and at a temperature of 30-110 ℃.
Further, in the steps S3-S4, the operation pressure of the washing tower is-0.015-0.025 MPaG, and the operation temperature is 20-100 ℃.
Further preferably, in the steps S3-S4, the operation pressure of the scrubbing tower is-0.010-0.020 MPaG, and the operation temperature is 30-90 ℃.
The second aspect of the present invention provides a system for hydrocyclone separation of ultra-high molecular weight polyethylene slurry, which is applied to the above-mentioned method for hydrocyclone separation of ultra-high molecular weight polyethylene slurry, and comprises:
a hydrocyclone separator;
the drier is connected with the hydrocyclone separator through a pipeline;
the washing tower is connected with the dryer through a pipeline;
and the condenser is connected with the washing tower and the dryer through pipelines.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the invention provides a method and a system for separating solid and liquid of slurry of ultra-high molecular polyethylene.A hydrocyclone is adopted to replace a centrifugal machine in the prior art to carry out solid-liquid separation on the slurry of polyethylene reaction, so that blocky materials and large-particle materials which originally cause the blockage of the centrifugal machine are settled to the bottom of the hydrocyclone, and are sent to a drier together with polyethylene wet cakes to carry out drying treatment; the technical scheme of the invention has simple process flow, continuous operation and low operation energy consumption, and the operation cycle of the UHMWPE device with the ultrahigh molecular weight is prolonged from 3-5 months of the centrifuge in the prior art to 18-20 months of the hydrocyclone separator, thereby obtaining better technical effect.
Drawings
FIG. 1 is a schematic process flow diagram of the hydrocyclone separation process for ultra-high molecular weight polyethylene slurry according to the present invention.
Detailed Description
The invention provides a method for separating ultra-high molecular weight polyethylene slurry by hydrocyclone, which can be applied to a large-scale commercial ultra-high molecular weight UHMWPE polyethylene industrial production device.
The invention also provides a system for separating the ultra-high molecular polyethylene slurry by hydrocyclone, which is applied to the method for separating the ultra-high molecular polyethylene slurry by hydrocyclone, and the centrifuge in the prior art is replaced by the hydrocyclone, and the blocky materials and the large-particle materials in the polyethylene slurry and the polyethylene wet cake are sent to the dryer together for drying treatment, thus better solving the problem that the centrifuge is blocked by the blocky materials and the large-particle materials in the prior art, and further the shutdown is caused.
The distribution of the sizes and the grain diameters of a certain grade of polyethylene particles in the existing ultrahigh molecular weight UHMWPE polyethylene production device is shown in the following table:
wherein: the polyethylene particles had an average particle size of 350 microns. Because the particle size of the UHMWPE polyethylene particles is more than 3 microns, the hydrocyclone is very suitable for the operation of a liquid-solid separation unit of polyethylene solid particles and hexane liquid solvent. According to the distribution condition of polyethylene particle size, the invention firstly adopts a hydrocyclone to replace the centrifuge in the prior art to carry out solid-liquid separation treatment on polyethylene slurry, and then uses a drier to carry out material drying treatment on the separated polyethylene wet cake to obtain dry polyethylene powder.
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
This example provides a method for hydrocyclone separation of ultra-high molecular weight polyethylene slurry, which is applied to a large-scale commercial ultra-high molecular weight UHMWPE polyethylene industrial production device, as shown in fig. 1, and the process flow thereof includes the following steps:
the hexane-containing ultra-high molecular weight UHMWPE polyethylene reaction slurry 1 from the upstream process enters a hydrocyclone 14; in the hydrocyclone 14, polyethylene reaction slurry 1 containing hexane enters the hydrocyclone 14 from a feeding pipe along a tangent line to form a rotational flow, the outer layer is a descending rotational flow, and polyethylene particles descend to polyethylene wet cake 2 containing hexane; the inner layer is an ascending cyclone, and the hexane liquid ascends to form the hexane solvent 4 without polyethylene particles.
The hexane 4 separated by the hydrocyclone 14 overflows from the upper part of the hydrocyclone 14, and the polyethylene wet cake 2 containing hexane separated by the hydrocyclone 14 falls through a head difference from the lower part of the hydrocyclone 14 into a dryer 15 for further drying.
Delivering the dried polyethylene powder 3 obtained in the dryer 15 to a subsequent granulation process, and allowing the nitrogen-containing hexane mixed gas 7 separated from the dryer 15 to enter a washing tower 16 for refining and purification and then to flow out from the top of the washing tower 16; the hexane 4 at the top of the washing column 16 is combined with the hexane 4 separated from the hydrocyclone 14 to form hexane 4, and the hexane 4 is sent to the hexane recovery process.
The dry nitrogen 5 from the outside is combined with the recycle stream 6 and enters a dryer 15, the polyethylene wet cake 2 is dried, the mixed gas 7 containing nitrogen and hexane flowing out of the dryer 15 enters a washing tower 16, the overhead stream 8 of the washing tower 16 flows into a condenser 17, the condensed hexane 4 flows back to the washing tower 16 in the condenser 17, one part of the stream 9 in the uncondensed nitrogen is combined with the dry nitrogen 5 and returns to the dryer 15 again, and the other part of the stream 9 is discharged to the outside.
Example 2
This example provides a system for hydrocyclone separation of ultra-high molecular weight polyethylene slurry based on the method described in example 1, applied to a large-scale commercial industrial production plant of ultra-high molecular weight UHMWPE polyethylene, comprising: a hydrocyclone 14; the dryer 15 is connected with the hydrocyclone 14 through a pipeline, and the cyclone separator 15 is connected with the cyclone separator 14 through a pipeline; a washing tower 16, wherein the washing tower 16 is connected with the dryer 15 through a pipeline; a condenser 17, wherein the condenser 17 is connected with the washing tower 16 and the dryer 15 through a pipeline.
This embodiment hydrocyclone separation ultra high molecular polyethylene slurry's system adopts hydrocyclone to replace prior art's centrifuge, and cubic material and large granule material in the polyethylene slurry send into the desiccator with the polyethylene wet cake together and carry out drying process, and better solution prior art has the centrifuge to be blocked by cubic material and large granule material, and then lead to the problem of parking. And the production capacity of the ultra-high molecular weight UHMWPE polyethylene production device adopting the hydrocyclone separation ultra-high molecular weight polyethylene slurry system can reach 1.0-15.0 ten thousand tons per year of large-scale commercial production.
Application comparative example 1
In the prior art, in the process of producing the UHMWPE polyethylene with the ultrahigh molecular weight, a centrifugal machine is adopted to carry out solid-liquid separation on slurry, and gaps of the centrifugal machine are easily blocked by massive materials and large-particle materials in the slurry polyethylene, so that the centrifugal machine is stopped and overhauled. Generally, the operating cycle of the prior art centrifuge is 3-5 months.
Application example 1
In the process, the UHMWPE slurry solid-liquid separation method uses the hydrocyclone separator to replace the original centrifuge to carry out solid-liquid separation on the slurry, and a disc dryer is used to further dry the separated wet cake. UHMWPE is produced on a scale of 1.0 ten thousand tons per year. The hydrocyclone was operated at a pressure of 0.050MPaG and an operating temperature of 70 ℃. The operating pressure of the disc dryer was 0.035MPaG and the operating temperature was 65 ℃. The operating pressure of the scrubber was 0.020MPaG and the operating temperature was 65 ℃.
The hydrocyclone of the invention is adopted to replace the centrifuge of the prior art, and the blocky materials and the large-particle materials in the polyethylene slurry and the polyethylene wet cake are sent to the dryer together for drying treatment, thereby better solving the problem that the centrifuge is blocked by the blocky materials and the large-particle materials, and the centrifuge stops in the prior art. Thus, the hydrocyclone of the present invention has an operating cycle of 18 months.
Application example 2
The UHMWPE production scale was 2.4 ten thousand tons/year as in application example 1. Except that the disc dryer was changed to a fluidized bed dryer. The operating pressure of the fluidized bed dryer was 0.025MPaG and the operating temperature was 80 ℃. Other equipment operating conditions were unchanged. Thus, the hydrocyclone of the present invention has an operating cycle of 19 months.
Application example 3
In the same way as in application example 1, the UHMWPE production scale was 15.0 ten thousand tons/year, 3 process lines. Except that the disc dryer was changed to a steam pot. The operating pressure of the steam pot was 0.015MPaG and the operating temperature was 60 ℃. Other equipment operating conditions were unchanged. Thus, the hydrocyclone of the present invention has an operating cycle of 20 months.
Compared with the application example and the application comparative example, the invention uses the hydrocyclone separator to replace the centrifuge in the prior art to carry out solid-liquid separation on the polyethylene reaction slurry, so that the blocky materials and the large-particle materials which are originally stuck by the centrifuge are settled to the bottom of the hydrocyclone separator and are sent to the dryer together with the polyethylene wet cake for drying treatment; the technical scheme of the invention has simple process flow, continuous operation and low operation energy consumption, and the operation cycle of the UHMWPE device with the ultrahigh molecular weight is prolonged from 3-5 months of the centrifuge in the prior art to 18-20 months of the hydrocyclone separator, thereby obtaining better technical effect.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. It will be appreciated by those skilled in the art that any equivalent modifications and substitutions are within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (10)
1. A method for separating ultra-high molecular weight polyethylene slurry by hydrocyclone is applied to a large-scale commercial ultra-high molecular weight UHMWPE polyethylene industrial production device, and is characterized by comprising the following steps:
s1, feeding the hexane-containing ultrahigh molecular weight UHMWPE polyethylene reaction slurry from the upstream process into a hydrocyclone; in the hydrocyclone separator, polyethylene reaction slurry containing hexane enters the hydrocyclone separator from a feeding pipe along a tangent line to form a rotational flow, the outer layer is a descending rotational flow, and polyethylene particles descend to form polyethylene wet cakes containing hexane; the inner layer is ascending rotational flow, and the hexane liquid ascends to form a hexane solvent without polyethylene particles;
s2, overflowing the hexane solvent separated by the hydrocyclone from the upper part of the dryer, and simultaneously falling the hexane-containing polyethylene wet cake separated by the hydrocyclone from the lower part of the dryer through a head difference into the dryer for further drying;
s3, conveying the dried polyethylene powder obtained in the dryer to a subsequent granulation process, and allowing the nitrogen-containing hexane mixed gas separated from the dryer to enter a washing tower, refining and purifying the nitrogen-containing hexane mixed gas and then allowing the nitrogen-containing hexane mixed gas to flow out from the top of the washing tower; the hexane at the top of the washing tower is combined with the hexane separated by the hydrocyclone into hexane which is sent to the hexane recovery process;
and S4, combining dry nitrogen from the outside with the circulating material flow, feeding the combined dry nitrogen and the circulating material flow into a dryer, drying the polyethylene wet cake, feeding the nitrogen-containing hexane mixed gas discharged from the dryer into a washing tower, feeding the material flow at the top of the washing tower into a condenser, refluxing hexane condensed in the condenser into the washing tower, combining one part of noncondensable nitrogen with the dry nitrogen, returning the combined dry nitrogen to the dryer again, and discharging the other part of material flow to the outside.
2. The method for hydrocyclone separation of an ultra high molecular weight polyethylene slurry according to claim 1, wherein:
in the step S1, the density of polyethylene particle solid in the polyethylene reaction slurry from the upstream process is 870-990 kg/cm3, the density of hexane solvent liquid is 500-850 kg/m3, the particle size of the UHMWPE polyethylene solid particle is 10-1500 microns, the average particle size of the particle is 100-700 microns, the hexane content is 50-80 wt%, and the content of polyethylene wet cake hexane separated by a hydrocyclone is 15-45 wt%;
in step S3, the content of hexane in the dried polyethylene powder flowing out of the dryer is 0.1-2.0 wt%.
3. The method for hydrocyclone separation of the ultra-high molecular polyethylene slurry according to claim 1, wherein the ultra-high molecular weight UHMWPE polyethylene production plant has a production capacity of 1.0-15.0 ten thousand tons per year for a large-scale commercial industrial plant.
4. The process for hydrocyclone separation of an ultra-high molecular weight polyethylene slurry according to claim 1, wherein in steps S1-S2, the hydrocyclone is operated at a pressure of 0.01-0.06 MPaG and at a temperature of 20-100 ℃.
5. The process for hydrocyclone separation of an ultra-high molecular weight polyethylene slurry according to claim 1, wherein the dryer is operated at a pressure of 0.002 to 0.042MPaG and at a temperature of 20 to 120 ℃ in steps S3 to S4; the mechanical structure of the dryer is one of a disc dryer, a fluidized bed dryer or a steam steaming tank.
6. The process for hydrocyclone separation of slurry of ultra-high molecular weight polyethylene according to claim 1, wherein the scrubber is operated at a pressure of-0.015 to 0.025MPaG and at a temperature of 20 to 100 ℃ in steps S3 to S4.
7. The process for hydrocyclone separation of an ultra-high molecular weight polyethylene slurry according to claim 4, wherein in steps S1-S2, the hydrocyclone is operated at a pressure of 0.02-0.05 MPaG and at a temperature of 30-90 ℃.
8. The process for hydrocyclone separation of the slurry of ultra-high molecular polyethylene according to claim 5, wherein in steps S3-S4, the dryer is preferably operated at a pressure of 0.007 to 0.037MPaG and at a temperature of 30 to 110 ℃.
9. The process for hydrocyclone separation of the slurry of ultra-high molecular weight polyethylene according to claim 6, wherein in steps S3-S4, the scrubbing column is operated at a pressure of-0.010 to 0.020MPaG and at a temperature of 30 to 90 ℃.
10. A system for hydrocyclone separation of an ultra high molecular weight polyethylene slurry for use in a method for hydrocyclone separation of an ultra high molecular weight polyethylene slurry as claimed in any one of claims 1 to 9, comprising:
a hydrocyclone separator;
the drier is connected with the hydrocyclone separator through a pipeline;
the washing tower is connected with the dryer through a pipeline;
and the condenser is connected with the washing tower and the dryer through pipelines.
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| CN114907505A (en) * | 2021-02-08 | 2022-08-16 | 中国科学院上海有机化学研究所 | Production process of ultrahigh molecular weight polyethylene |
| CN115838450A (en) * | 2021-09-18 | 2023-03-24 | 中国石油化工股份有限公司 | Preparation method for slurry polyethylene |
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