CN115838450B - Preparation method for slurry polyethylene - Google Patents
Preparation method for slurry polyethylene Download PDFInfo
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- CN115838450B CN115838450B CN202111097982.7A CN202111097982A CN115838450B CN 115838450 B CN115838450 B CN 115838450B CN 202111097982 A CN202111097982 A CN 202111097982A CN 115838450 B CN115838450 B CN 115838450B
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- 239000002002 slurry Substances 0.000 title claims abstract description 177
- 239000004698 Polyethylene Substances 0.000 title claims abstract description 34
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 34
- -1 polyethylene Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 59
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005977 Ethylene Substances 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 29
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000000498 cooling water Substances 0.000 claims description 9
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 239000007788 liquid Substances 0.000 abstract description 17
- 238000006116 polymerization reaction Methods 0.000 description 31
- 229920001903 high density polyethylene Polymers 0.000 description 15
- 239000004700 high-density polyethylene Substances 0.000 description 15
- 239000011259 mixed solution Substances 0.000 description 15
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 14
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 14
- 239000000463 material Substances 0.000 description 7
- 229920000092 linear low density polyethylene Polymers 0.000 description 6
- 239000004707 linear low-density polyethylene Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 229920010126 Linear Low Density Polyethylene (LLDPE) Polymers 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000002902 bimodal effect Effects 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- 229920001179 medium density polyethylene Polymers 0.000 description 2
- 239000004701 medium-density polyethylene Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a preparation method for slurry polyethylene, which comprises the following steps: feeding ethylene monomer, catalyst, solvent into a first slurry reactor; dividing the primary slurry mixture into a primary tributary slurry mixture, a secondary tributary slurry mixture, and a tertiary tributary slurry mixture; and (3) the slurry mixed liquid of each branch is subjected to different reaction flows, and finally, the converged slurry mixed liquid is reacted and then passes through a second devolatilizer and a second axial flow pump to obtain a polyethylene product. The invention adopts the slurry mixed liquid to split, so that the slurry mixed liquid of each tributary passes through different reaction flows and the number of slurry reactors, the problem of poor flexibility of slurry polyethylene reaction equipment is effectively solved, and a set of equipment is used for producing various polyethylene products.
Description
Technical Field
The invention relates to the field of polymers, in particular to a preparation method for slurry polyethylene.
Background
Polyethylene (PE) is the most productive species among general synthetic resins, and the products include: low Density Polyethylene (LDPE), linear Low Density Polyethylene (LLDPE), medium Density Polyethylene (MDPE), high Density Polyethylene (HDPE), ultra high molecular weight polyethylene (UHWPE), and the like. At present, the international polyethylene resin market competition is strong, the middle east country is in the market of preempting polyethylene general-purpose materials in large quantities by virtue of the cost advantage, and petrochemical enterprises in the countries and regions of the United states, europe, japan and the like are accelerating the development and production of polyethylene high-grade materials and special materials.
The preparation method of the polyethylene mainly comprises a slurry method, a gas phase method, a solution method and the like, wherein the slurry polymerization process is relatively mature as an early industrialization technology, and has the advantages of low reaction temperature and pressure, high single-pass conversion rate of ethylene, easy control of operation conditions, good product performance and wide application in the field of preparing the polyethylene.
The application of patent application No. 201911235641.4 discloses a bimodal high density polyethylene and a process for producing the same, which is produced by contacting ethylene and at least one (C4-C20) alpha-olefin with a bimodal catalyst in a single gas phase reactor in the presence of hydrogen and an Induced Condensing Agent (ICA), the comonomer content and the polymer yield being adjusted by adjusting the content of hydrogen and the induced condensing agent in the reactor.
The existing slurry polyethylene preparation method has poor flexibility, and a set of expensive polyethylene equipment can be used for producing a plurality of polyethylene products with fixed marks, and the copolymer type and yield can be adjusted only by adjusting the reaction temperature, the reaction pressure and the hydrogen and the content of an induced condensing agent in a reactor.
Disclosure of Invention
The invention aims to: the invention aims to provide a preparation method for slurry polyethylene, which has the advantages of free production flow switching, flexible operation and simple process flow.
The technical scheme is as follows: a process for the preparation of a slurry polyethylene, the process comprising the steps of:
(a) Feeding ethylene monomer, catalyst, solvent into a first slurry reactor; polymerizing the ethylene monomer, catalyst, solvent in the primary slurry reactor, thereby producing a primary slurry mixture;
(b) Dividing the primary slurry mixture into a primary tributary slurry mixture, a secondary tributary slurry mixture, and a tertiary tributary slurry mixture;
(c) The first tributary slurry mixed liquor is fed to the second slurry reactor through a first devolatilizer and a first axial flow pump;
(d) The second tributary slurry mixed liquor is fed into a second slurry reactor, and polymerization is carried out on the second tributary slurry mixed liquor, the first tributary slurry mixed liquor, ethylene monomer, catalyst and solvent in the second slurry reactor;
(e) The third subsidiary slurry mixture and the second slurry mixture are passed through a second devolatilizer and a second axial flow pump to produce a polyethylene product.
Further, the primary slurry reactor and secondary slurry reactor are operated at the same temperature and pressure conditions.
Further, prior to step (b), the primary slurry mixture is reacted by passing through n slurry reactors in series, where n is less than or equal to 4.
Further, the primary slurry mixture in step (b) is split by a splitting device, which is one or more of a regulating valve, a venturi tube or a restriction orifice.
Further, prior to said step (b), said primary slurry mixture is subjected to heat removal by a primary heat remover, and unreacted ethylene in the primary slurry reactor is recycled to the primary slurry reactor through the primary heat remover.
Further, before the step (e), the secondary slurry mixed solution is subjected to heat removal through a secondary heat remover, and unreacted ethylene in the secondary slurry reactor is recycled to the secondary slurry reactor through the primary heat remover.
Further, in the step (a), the primary slurry mixture is stirred by a stirrer in the primary slurry reactor. In step (d), the secondary slurry mixture is stirred by a stirrer in the secondary slurry reactor.
Further, in the step (a), the primary slurry mixture is subjected to heat removal through a jacket of the primary slurry reactor, and circulating cooling water is contained in the jacket; in the step (d), the secondary slurry mixed liquid is subjected to heat removal through a jacket of the secondary slurry reactor, and circulating cooling water is contained in the jacket;
further, the top of the first devolatilizer and/or the second devolatilizer is provided with an exhaust pipe, and the volatile gas generated in the first devolatilizer and/or the second devolatilizer is discharged from the exhaust pipe.
Further, the first tributary slurry mixture accounts for 0-100 wt% of the first slurry mixture, the second tributary slurry mixture accounts for 0-100 wt% of the first slurry mixture, and the third tributary slurry mixture accounts for 0-100 wt% of the first slurry mixture.
The beneficial effects are that: compared with the prior art, the invention has the remarkable technical effects that:
1. the flexibility of the reaction equipment is high, the slurry mixed liquid is split, so that the slurry mixed liquid of each branch flows through different reaction processes and the number of slurry reactors, the problem of poor flexibility of the slurry polyethylene reaction equipment is effectively solved, and a set of equipment is used for producing various polyethylene products.
2. The reaction flow is effectively simplified, and the slurry reactors adopt the same operation conditions of reaction materials, temperature, pressure and the like, so that the flow of the preparation method is effectively simplified.
3. The reaction condition is controllable, and the heat of reaction is effectively reduced due to the addition of the heat remover and the jacket with circulating cooling water, so that the reaction condition is controllable.
4. The serial-parallel switching is free, and the slurry mixed liquid is split to realize the content adjustment of the tributary slurry mixed liquid, so that the reaction flow is conveniently switched between serial connection and parallel connection.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
Example 1
Taking a linear low density polyethylene LLDPE device with a nominal capacity of 25 ten thousand tons/year as an example, the process for preparing a slurry polyethylene according to the present invention is employed.
As shown in fig. 1, the process flow of this embodiment is as follows: (a) Ethylene monomer 1, catalyst 2 and solvent 3 are fed into a first slurry reactor A1 for polymerization reaction to generate a first slurry mixed solution 5, the slurry reactor A1 is provided with a stirrer and a jacket, wherein the stirrer ensures that reaction materials are uniformly mixed, one part of reaction heat is removed by jacket circulating cooling water, the other part of reaction heat is removed by a slurry external circulation by circulating cooling water of a heat remover B1, and circulating ethylene 4 is returned to the slurry reactor A1; the primary slurry mixture 5, before being split, flows through n slurry reactors in series, n being equal to 1; (b) The primary slurry mixture 5 is divided into a primary tributary slurry mixture 6, a secondary tributary slurry mixture 7, and a tertiary tributary slurry mixture 8, wherein the primary tributary slurry mixture has a proportion M1 of 25wt% in the primary slurry mixture, the secondary tributary slurry mixture has a proportion M2 of 35wt% in the primary slurry mixture, and the tertiary tributary slurry mixture has a proportion M3 of 40wt% in the primary slurry mixture, namely M1: m2: m3=25: 35:40, a step of performing a; (c) The first tributary slurry mixed solution 6 enters a first devolatilizer C1, is stirred and separated by a stirrer in the first devolatilizer C1, and volatile gas 13 is discharged out of the boundary through a first exhaust pipe D1; (d) The first tributary slurry mixed liquor 6 is pressurized by a first axial flow pump E1 to generate mixed liquor 9, the mixed liquor 9, a second tributary slurry mixed liquor 7, ethylene monomers 10, a catalyst 11 and a solvent 12 are fed into a second slurry reactor A2 to carry out polymerization reaction to generate a second slurry mixed liquor 14, the slurry reactor A2 is provided with a stirrer and a jacket, wherein the stirrer ensures that reaction materials are uniformly mixed, one part of reaction heat is removed by jacket circulating cooling water, the other part of reaction heat is removed by the heat remover B2 circulating cooling water through slurry external circulation, and circulating ethylene 15 is returned to the slurry reactor A2; (e) The third branch slurry mixed solution 8 and the second slurry mixed solution 14 enter a second devolatilizer C2 and a second axial flow pump E2 to obtain a polyethylene product 16, the third branch slurry mixed solution 8 and the second slurry mixed solution 14 are stirred and separated by a stirrer in the second devolatilizer C2, and the volatile gas 17 is discharged out of the boundary through a second exhaust pipe D2.
The process operating parameters of this example are as follows: the reaction conditions of each slurry reactor were the same, the polymerization temperature was 105 ℃, the polymerization pressure was 4.2MPaA, and the polymerization time was 2.0 hours.
The Linear Low Density Polyethylene (LLDPE) produced has a density of 0.918 to 0.935g/cm 3 The molecular weight is 10,000-100,000.
Example 2
Compared with the example 1, only nominal capacity, the proportion of each branch of the slurry mixed liquid and the operation parameters of the process are changed, and the nominal capacity is 20 ten thousand tons/year of high-density polyethylene HDPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=20: 30:50; the process operating parameters of this example were modified as follows: the polymerization temperature was 110℃and the polymerization pressure was 4.6MPaA, and the polymerization time was 3.0 hours.
The density of the produced High Density Polyethylene (HDPE) is 0.941-0.960g/cm3, and the molecular weight is 40,000-300,000.
Example 3
Compared with the example 1, only nominal capacity, the proportion of each branch of the slurry mixed liquid and the operation parameters of the process are changed, and the nominal capacity is 10 ten thousand tons/year of ultra-high molecular weight polyethylene UHWPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=22: 36:42; the process operating parameters of this example were modified as follows: the polymerization temperature was 78 ℃, the polymerization pressure was 3.8MPaA, and the polymerization time was 0.5 hour.
The density of the produced ultra-high molecular weight polyethylene (UHWPE) is 0.920-0.964g/cm3, and the molecular weight is more than 1,500,000.
Example 4
Compared with the example 1, only nominal capacity, the ratio of each branch of the slurry mixed liquid, the number of slurry reactors connected in series and the operation parameters of the process are changed, wherein the nominal capacity is 40 ten thousand tons/year of linear low-density polyethylene LLDPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=55: 20:25, a step of selecting a specific type of material; the number n of the slurry reactors connected in series is 2; the process operating parameters of this example were modified as follows: the polymerization temperature was 168℃and the polymerization pressure was 7.6MPaA, and the polymerization time was 6.0 hours.
The Linear Low Density Polyethylene (LLDPE) produced has a density of 0.918-0.935g/cm3 and a molecular weight of 10,000-100,000.
Example 5
Compared with the example 1, only nominal capacity, the ratio of each branch of the slurry mixed liquid, the number of slurry reactors connected in series and the operation parameters of the process are changed, wherein the nominal capacity is 50 ten thousand tons/year of high-density polyethylene HDPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=60: 25:15; the number n of the slurry reactors connected in series is 3; the process operating parameters of this example were modified as follows: the polymerization temperature was 170℃and the polymerization pressure was 6.8MPaA, and the polymerization time was 1.5 hours.
The density of the produced High Density Polyethylene (HDPE) is 0.941-0.960g/cm3, and the molecular weight is 40,000-300,000.
Example 6
Compared with the example 1, only nominal capacity, the ratio of each branch of the slurry mixed liquid, the number of slurry reactors connected in series and the operation parameters of the process are changed, wherein the nominal capacity is 15 ten thousand tons/year ultra-high molecular weight polyethylene UHWPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=66: 14:20, a step of; the number n of the slurry reactors connected in series is 2; the process operating parameters of this example were modified as follows: the polymerization temperature was 166℃and the polymerization pressure was 9.0MPaA, and the polymerization time was 4.5 hours.
The density of the produced ultra-high molecular weight polyethylene (UHWPE) is 0.920-0.964g/cm3, and the molecular weight is more than 1,500,000.
Example 7
Compared with the example 1, only nominal capacity, the ratio of each branch of the slurry mixed liquid, the number of slurry reactors connected in series and the operation parameters of the process are changed, wherein the nominal capacity is 5 ten thousand tons/year of ultra-high molecular weight polyethylene UHWPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=0: 0:100; the number n of the slurry reactors connected in series is 0; the process operating parameters of this example were modified as follows: the polymerization temperature was 50℃and the polymerization pressure was 0.2MPaA, and the polymerization time was 3.2 hours.
The density of the produced ultra-high molecular weight polyethylene (UHWPE) is 0.920-0.964g/cm3, and the molecular weight is more than 1,500,000.
Example 8
Compared with the example 1, only nominal capacity, the ratio of each branch of the slurry mixed liquid, the number of slurry reactors connected in series and the operation parameters of the process are changed, wherein the nominal capacity is 60 ten thousand tons/year linear low-density polyethylene LLDPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=0: 100:0; the number n of the slurry reactors connected in series is 0; the process operating parameters of this example were modified as follows: the polymerization temperature was 50℃and the polymerization pressure was 10.2MPaA, and the polymerization time was 3.4 hours.
The Linear Low Density Polyethylene (LLDPE) produced has a density of 0.918-0.935g/cm3 and a molecular weight of 10,000-100,000.
Example 9
Compared with the example 1, only nominal capacity, the ratio of each branch of the slurry mixed liquid, the number of slurry reactors connected in series and the operation parameters of the process are changed, wherein the nominal capacity is 60 ten thousand tons/year of high-density polyethylene HDPE device; the ratio of each tributary of the slurry mixed solution is M1: m2: m3=100: 0:0; the number n of the slurry reactors connected in series is 4; the process operating parameters of this example were modified as follows: the polymerization temperature was 200℃and the polymerization pressure was 10.2MPaA, and the polymerization time was 3.6 hours.
The density of the produced High Density Polyethylene (HDPE) is 0.941-0.960g/cm3, and the molecular weight is 40,000-300,000.
Claims (10)
1. A process for the preparation of a slurry polyethylene, said process comprising the steps of:
(a) Feeding ethylene monomer, catalyst, solvent into a first slurry reactor; polymerizing the ethylene monomer, catalyst, solvent in the primary slurry reactor, thereby producing a primary slurry mixture;
(b) Dividing the primary slurry mixture into a primary tributary slurry mixture, a secondary tributary slurry mixture, and a tertiary tributary slurry mixture;
(c) The first tributary slurry mixed liquor is fed to the second slurry reactor through a first devolatilizer and a first axial flow pump;
(d) Feeding the second subsidiary slurry mixture to a second slurry reactor in which the second subsidiary slurry mixture, the first subsidiary slurry mixture, the ethylene monomer, the catalyst, and the solvent polymerize to thereby produce a second slurry mixture;
(e) The third subsidiary slurry mixture and the second slurry mixture are passed through a second devolatilizer and a second axial flow pump to produce a polyethylene product.
2. The process for the preparation of slurry polyethylene according to claim 1, characterized in that the primary slurry reactor and the secondary slurry reactor are operated under the same temperature and pressure conditions.
3. The process for preparing a slurry polyethylene according to claim 1, wherein said primary slurry mixture is reacted by passing through n slurry reactors in series, n being less than or equal to 4, before said step (b).
4. The method for preparing a slurry polyethylene according to claim 1, wherein the primary slurry mixture in said step (b) is split by a splitting means, which is one or more of a regulating valve, a venturi tube or a restriction orifice plate.
5. The process for preparing a slurry polyethylene according to claim 1, wherein prior to said step (b), the primary slurry mixture is subjected to heat removal by a primary heat remover, and unreacted ethylene in the primary slurry reactor is circulated to the primary slurry reactor through the primary heat remover.
6. The process for preparing a slurry polyethylene according to claim 1, wherein prior to said step (e), the secondary slurry mixture is subjected to heat removal by a secondary heat remover, and unreacted ethylene in the secondary slurry reactor is recycled to the secondary slurry reactor through said secondary heat remover.
7. The process for preparing a slurry polyethylene according to claim 1, wherein in said step (a), said primary slurry mixture is stirred by a stirrer in a primary slurry reactor; in step (d), the secondary slurry mixture is stirred by a stirrer in the secondary slurry reactor.
8. The process for preparing a slurry polyethylene according to claim 1, wherein in said step (a), said primary slurry mixture is heat removed through a jacket of a primary slurry reactor, said jacket containing circulating cooling water; in the step (d), the secondary slurry mixture is heat removed through a jacket of the secondary slurry reactor, the jacket containing circulating cooling water.
9. The method for producing a slurry polyethylene according to claim 1, wherein said first devolatilizer and/or said second devolatilizer are/is provided at the top with an exhaust pipe from which the volatile gas generated in the first devolatilizer and/or the second devolatilizer is discharged.
10. The method for producing a slurry polyethylene according to claim 1, wherein the first tributary slurry mixture is 0 to 100wt% of the first slurry mixture, the second tributary slurry mixture is 0 to 100wt% of the first slurry mixture, and the third tributary slurry mixture is 0 to 100wt% of the first slurry mixture.
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