CN108329429B - Method for continuously preparing light-colored dicyclopentadiene petroleum resin - Google Patents
Method for continuously preparing light-colored dicyclopentadiene petroleum resin Download PDFInfo
- Publication number
- CN108329429B CN108329429B CN201810186351.4A CN201810186351A CN108329429B CN 108329429 B CN108329429 B CN 108329429B CN 201810186351 A CN201810186351 A CN 201810186351A CN 108329429 B CN108329429 B CN 108329429B
- Authority
- CN
- China
- Prior art keywords
- polymerization
- dicyclopentadiene
- liquid
- petroleum resin
- 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
- C08F240/00—Copolymers of hydrocarbons and mineral oils, e.g. petroleum resins
-
- 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
-
- 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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/04—Reduction, e.g. hydrogenation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
Abstract
The invention relates to a method for continuously preparing light-color dicyclopentadiene petroleum resin, which comprises the following steps: the dicyclopentadiene monomer and the polymerization solvent are continuously fed into a polymerization kettle to prepare the dicyclopentadiene petroleum resin through thermal polymerization, and the obtained polymerization reaction liquid is directly subjected to continuous hydrogenation. And (3) removing the solvent from the hydrogenation reaction liquid through flash evaporation, removing the oligomer in a reduced pressure distillation tower, and finally cooling to obtain the solid light-colored petroleum resin. The method shortens the process flow, has simple and convenient equipment, particularly adopts continuous single kettle thermal polymerization, reduces the equipment investment cost, simplifies the process control operation, ensures that the obtained polymerization reaction liquid directly enters a hydrogenation device, effectively shortens the production period by about 20 percent, reduces the energy consumption and increases the benefit.
Description
Technical Field
The invention relates to the field of high polymer synthesis, in particular to a method for preparing light-colored dicyclopentadiene petroleum resin.
Background
The dicyclopentadiene petroleum resin is obtained by thermally polymerizing dicyclopentadiene which is obtained by separating a byproduct generated in the preparation of olefin through petroleum cracking and has higher purity. The resin has high unsaturation degree and poor oxidation stability, is not suitable for direct use, can saturate double bonds in the resin through hydrogenation to obtain light-colored resin with good light resistance and thermal property, and can be used as a hot melt adhesive or a pressure-sensitive adhesive, thereby expanding the application range of the resin.
Patent CN101003602 discloses a process for producing C9 petroleum resin by multi-kettle series continuous thermal polymerization, which mainly comprises the steps of carbon nine raw material purification pretreatment, multi-kettle series thermal polymerization, feeding the polymerized material into a first-level evaporator and then into a second-level falling film flash evaporator, and finally slicing and cooling.
Patent CN102516461 discloses a preparation method of light-colored high-softening-point hydrogenated dicyclopentadiene petroleum resin, which mainly comprises the steps of dissolving a resin raw material in a selected solvent again, removing impurities by an adsorption tower, and then entering a fixed bed reactor for catalytic hydrogenation. The catalyst is a special nickel-zinc-silicon bimetallic catalyst.
The polymerization section and the hydrogenation section in the technology are two-section independent processes, the polymerization section adopts a multi-kettle series continuous polymerization process with complicated equipment, the solvent and the oligomer of the polymerization reaction liquid need to be removed to control the softening point of the product, the molten base petroleum resin is obtained, and the molten base petroleum resin is dissolved in the hydrogenation solvent and then enters the hydrogenation process section, and the whole process is complicated.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for continuously preparing light-color dicyclopentadiene petroleum resin, which can continuously hydrogenate polymerization reaction liquid without removing a solvent.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for continuously preparing the light-color dicyclopentadiene petroleum resin is characterized by comprising the following steps:
continuously feeding a dicyclopentadiene raw material and an inert solvent into a polymerization kettle for thermal polymerization, controlling the reaction temperature in the polymerization kettle to be 220-270 ℃, the reaction pressure to be 0.5-2.0 MPa, the liquid level in the polymerization kettle to be 60-80%, and the retention time of materials to be 0.5-20.0 h; obtaining a polymerization reaction liquid at an outlet of the polymerization kettle;
controlling the amount of the inert solvent in the reaction system in the polymerization kettle to be 55-85 wt% of the total amount of the reaction raw materials;
the inert solvent is at least one selected from aromatic hydrocarbon, naphthenic hydrocarbon, straight-chain alkane, dearomatized aliphatic hydrocarbon and isoparaffin;
conveying the obtained polymerization reaction liquid to a first flash tank for flash evaporation to remove unreacted monomers accounting for 0.5-4.0 wt% of the monomer raw materials, filtering out colloids and other impurities by using a 100-400-mesh filter screen filter, and then feeding the obtained polymerization reaction liquid into a hydrogenation reactor; controlling the reaction conditions of the hydrogenation reactor as follows: the reaction pressure is 6.0-15.0 MPa, the reaction temperature is 200-280 ℃, and the volume airspeed is 0.3-1.0 h～1The hydrogen-oil ratio is 500: 1-1000: 1; the hydrogenation catalyst is a supported palladium catalyst, and the mass fraction of PdThe number of the catalyst is 0.5-2.0%, the catalyst carrier is gamma-Al 2O3, and the specific surface area is 80-250 m2/g；
The hydrogenated resin liquid obtained after hydrogenation is conveyed to a second flash tank to be evaporated to obtain a flash-evaporated resin liquid; controlling the flash evaporation temperature to be 170-200 ℃ and the flash evaporation pressure to be 80-200 kPa;
and (3) conveying the flash evaporation resin liquid to a distillation tower for reduced pressure distillation, controlling the temperature of the top of the distillation tower to be 180-220 ℃ and the operating pressure to be 10-20 kPa, discharging the oligomer from the top of the distillation tower, and obtaining the light-colored dicyclopentadiene petroleum resin at the bottom of the distillation tower.
Preferably, the dicyclopentadiene raw material can be a petroleum cracking C5 mixture, and the dicyclopentadiene content in the dicyclopentadiene raw material is 67-87 wt%.
The inert solvent in each scheme can be any one of the prior arts according to needs, and preferably can be at least one selected from benzene, toluene, xylene, trimethylbenzene, hexane, cyclohexane, heptane, octane, nonane, decane, undecane, dodecane, No. 100 solvent oil, No. 200 solvent oil, solvent D40, solvent D60, Isopar H and Isopar L.
Furthermore, a gas phase outlet at the top of the polymerization kettle can be sequentially connected with a condenser and a liquid distributor, after gas phase substances in the polymerization kettle are introduced into the condenser through a pipeline for condensation, separated liquid phase and the cyclopentadiene raw material enter a static mixer for mixing, and then enter the polymerization kettle from the lower part of the polymerization kettle.
Further, an inert solvent can be supplemented into the polymerization reaction liquid of the polymerization kettle, and the mixture is uniformly mixed and then enters a hydrogenation reactor; the amount of the added inert solvent is 0.5 to 5.0 wt% of the polymerization reaction solution. To further improve the quality of the product.
Compared with the prior art, the method for continuously preparing the light-color dicyclopentadiene petroleum resin not only simplifies the polymerization section into single-kettle continuous polymerization, but also ensures that the polymerization reaction liquid can directly enter the continuous hydrogenation section without removing the polymerization solvent, thereby saving the process link of removing the polymerization solvent, simplifying the process operation flow, effectively shortening the production period by about 20 percent, realizing energy conservation and consumption reduction, reducing environmental pollution, reducing the equipment investment cost, having simple and convenient process, reducing the equipment investment and obtaining a product with good color phase.
Drawings
Fig. 1 is a schematic flow chart of embodiment 1 of the present invention.
Wherein:
1. a polymerization kettle; 2. a condenser; 3. a liquid separator; 4. 12, a static mixer; 5. 8, 11, a delivery pump; 6. a feed valve; 7. a discharge valve; 9. 13, a heat exchanger; 10. a first flash tank; 14. a hydrogenation reactor; 15. a second flash tank; 16. a distillation column.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The hydrogenation catalysts used in examples 1 to 4 are all supported palladium catalysts, the mass fraction of Pd is 1.0%, and the catalyst carrier is gamma-Al2O3A specific surface area of 220m2/g。
Example 1
As shown in figure 1, dicyclopentadiene and trimethylbenzene inert solvent are mixed according to the weight ratio of 35:65 and then are put into a polymerization kettle 1, the liquid level is stabilized at 70%, when the temperature is slowly raised to 270 ℃ at the speed of 2-3 ℃/min, a feeding valve and a discharging valve are opened, and the retention time of polymerization reaction raw materials is controlled to be 0.7h by the opening degree of the discharging valve and the liquid level in the kettle.
Unreacted gas-phase reaction raw materials discharged from a gas-phase outlet at the top of the polymerization kettle enter a condenser 2 through a pipeline, the gas-phase reaction raw materials are condensed to 20-30 ℃, then the condensed gas-phase reaction raw materials enter a liquid separator 3, and separated liquid phases and cyclopentadiene raw materials enter a static mixer 4 to be mixed and then are sent into the polymerization kettle 1 from the lower part of the polymerization kettle by a pump 5.
The polymerization reaction liquid obtained at the bottom of the polymerization kettle is continuously sent to a first flash tank 10 by a pump 8, unreacted monomers accounting for 1.5 wt% of the monomer raw materials are removed under normal pressure, colloid and other impurities are filtered by a 100-mesh filter screen filter, and then the unreacted monomers and inert solvent which is supplemented by a pipeline and accounts for 2.0 wt% of the polymerization reaction liquid enter a static mixer 12 to be mixed, and the mixture is subjected to reactionThe heat exchanger 13 exchanges heat to 200 ℃, and the obtained product is continuously conveyed to the hydrogenation and decolorization reactor 14. The hydrogen enters the catalyst bed layer together with the polymerization reaction liquid after being pressurized by the compressor, the reaction temperature in the hydrogenation and decoloration reactor 14 is controlled to be 250 ℃, the reaction pressure is controlled to be 15MPa, and the volume airspeed is controlled to be 0.5h～1The hydrogen-oil ratio is 600: 1.
The reaction liquid after the hydrogenation and the decoloration enters a second flash tank 15 for flash evaporation; and controlling the flash evaporation temperature in the second flash tank to be 200 ℃ and the operation pressure to be 140 kPa. Obtaining the inert solvent at the top of the second flash tank, and pumping the inert solvent to a polymerization solvent storage tank through a recovery pump for recycling of the polymerization reaction.
Obtaining hydrogenated resin liquid at the bottom of the second flash tank, and sending the hydrogenated resin liquid to a reduced pressure distillation tower 16 for continuously removing oligomers; controlling the tower top temperature of the distillation tower to be 200 ℃ and the operating pressure to be 10 kPa; discharging the oligomer from the top of the distillation tower, obtaining molten resin from the bottom of the distillation tower, and cooling to obtain solid light-colored dicyclopentadiene petroleum resin. The softening point was measured to be 112 ℃ and the Gardener colour was < 1.
Example 2
As shown in fig. 1, dicyclopentadiene and cyclohexane were mixed in a weight ratio of 25: 75, putting the mixture into a polymerization kettle 1, stabilizing the liquid level at 75%, slowly heating to 260 ℃ at the speed of 2-3 ℃/min, opening a feed valve and a discharge valve, and controlling the retention time of the polymerization reaction raw materials to be 2.5h by the opening degree of the discharge valve and the liquid level in the kettle.
And unreacted gas-phase reaction raw materials discharged from a gas-phase outlet at the top of the polymerization kettle enter a condenser through a pipeline, the gas-phase reaction raw materials are condensed to 20-30 ℃, then the gas-phase reaction raw materials enter a liquid separator, and the separated liquid phase and the cyclopentadiene raw materials enter a static mixer to be mixed and then enter the polymerization kettle from the lower part of the polymerization kettle.
The polymerization reaction liquid obtained at the bottom of the polymerization kettle is continuously pumped to a first flash tank 10, unreacted monomers accounting for 1.0 wt% of the monomer raw materials are removed under normal pressure, colloid and other impurities are filtered by a 400-mesh filter screen, and then the polymerization reaction liquid and inert solvent which is supplemented by a pipeline and accounts for 2.0 wt% of the polymerization reaction liquid enter a second static mixer 12 to be mixed, heat is exchanged to 100 ℃ through a heat exchanger 13, and the mixture is continuously conveyed to a hydrogenation and decoloration reactor 14. Hydrogen gasThe reaction liquid enters a catalyst bed layer together with polymerization reaction liquid after being pressurized by a compressor, the reaction temperature in a hydrogenation and decoloration reactor 14 is controlled to be 200 ℃, the reaction pressure is controlled to be 12MPa, and the volume airspeed is controlled to be 0.3h～1Hydrogen to oil ratio 900: 1.
The reaction liquid after the hydrogenation and the decoloration enters a second flash tank 15 for flash evaporation; and controlling the flash evaporation temperature in the second flash evaporation tank to be 180 ℃ and the operation pressure to be 100 kPa. Obtaining the inert solvent at the top of the second flash tank, and pumping the inert solvent to a polymerization solvent storage tank through a recovery pump for recycling of the polymerization reaction.
Obtaining hydrogenated resin liquid at the bottom of the second flash tank, and sending the hydrogenated resin liquid to a reduced pressure distillation tower 16 for continuously removing oligomers; controlling the tower top temperature of the distillation tower to be 180 ℃ and the operating pressure to be 10 kPa; discharging the oligomer from the top of the distillation tower, obtaining molten resin from the bottom of the distillation tower, and cooling to obtain solid light-colored dicyclopentadiene petroleum resin. The softening point of the resin is tested to be 104 ℃ and the Gardener color is less than 1.
Example 3
As shown in figure 1, dicyclopentadiene and 200 # solvent oil are mixed according to a weight ratio of 45: 55, putting the mixture into a polymerization kettle 1, stabilizing the liquid level at 60%, slowly heating to 250 ℃ at the speed of 2-3 ℃/min, opening a feed valve and a discharge valve, and controlling the retention time of the polymerization reaction raw materials to be 7h by the opening degree of the discharge valve and the liquid level in the kettle.
And unreacted gas-phase reaction raw materials discharged from a gas-phase outlet at the top of the polymerization kettle enter a condenser through a pipeline, the gas-phase reaction raw materials are condensed to 20-30 ℃, then the gas-phase reaction raw materials enter a liquid separator, and the separated liquid phase and the cyclopentadiene raw materials enter a static mixer to be mixed and then enter the polymerization kettle from the lower part of the polymerization kettle.
The polymerization reaction liquid obtained at the bottom of the polymerization kettle is continuously pumped to a first flash tank 10, unreacted monomers accounting for 3.0 wt% of the monomer raw materials are removed under normal pressure, colloid and other impurities are filtered by a 200-mesh filter screen filter, and then the polymerization reaction liquid and inert solvent which is supplemented by a pipeline and accounts for 5.0 wt% of the polymerization reaction liquid enter a second static mixer 12 to be mixed, heat is exchanged to 130 ℃ through a heat exchanger 13, and the mixture is continuously conveyed to a hydrogenation and decoloration reactor 14. Pressurizing hydrogen by compressor, feeding the pressurized hydrogen and polymerization reaction liquid into catalyst bed layer together, and controllingThe reaction temperature in the hydrogenation and decoloration reactor 14 is 230 ℃, the reaction pressure is 10MPa, and the volume space velocity is 0.7h～1Hydrogen to oil ratio of 700: 1.
The reaction liquid after the hydrogenation and the decoloration enters a second flash tank 15 for flash evaporation; the flash evaporation temperature in the second flash evaporation tank is controlled to be 250 ℃, and the operation pressure is controlled to be 100 kPa. Obtaining the inert solvent at the top of the second flash tank, and pumping the inert solvent to a polymerization solvent storage tank through a recovery pump for recycling of the polymerization reaction.
Obtaining hydrogenated resin liquid at the bottom of the second flash tank, and sending the hydrogenated resin liquid to a reduced pressure distillation tower 16 for continuously removing oligomers; controlling the tower top temperature of the distillation tower to be 200 ℃ and the operating pressure to be 15 kPa; discharging the oligomer from the top of the distillation tower, obtaining molten resin from the bottom of the distillation tower, and cooling to obtain solid light-colored dicyclopentadiene petroleum resin. The softening point of the product is 110 ℃ and the Gardener color is less than 1.
Example 4
As shown in fig. 1, dicyclopentadiene and Isopar L inert solvent were mixed in a weight ratio of 15: 85, the mixture is put into a polymerization kettle 1, the liquid level is stabilized at 80 percent, when the temperature is slowly raised to 245 ℃ at the speed of 2-3 ℃/min, a feed valve and a discharge valve are opened, and the retention time of the polymerization reaction raw materials is controlled to be 20 hours by the opening degree of the discharge valve and the liquid level in the kettle.
And unreacted gas-phase reaction raw materials discharged from a gas-phase outlet at the top of the polymerization kettle enter a condenser through a pipeline, the gas-phase reaction raw materials are condensed to 20-30 ℃, then the gas-phase reaction raw materials enter a liquid separator, and the separated liquid phase and the cyclopentadiene raw materials enter a static mixer to be mixed and then enter the polymerization kettle from the lower part of the polymerization kettle.
The polymerization reaction liquid obtained at the bottom of the polymerization kettle is continuously pumped to a first flash tank 10, unreacted monomers accounting for 2.0 wt% of the monomer raw materials are removed under normal pressure, colloid and other impurities are filtered by a 300-mesh filter screen filter, and then the polymerization reaction liquid and inert solvent which is supplemented by a pipeline and accounts for 2.0 wt% of the polymerization reaction liquid enter a second static mixer 12 to be mixed, heat is exchanged to 170 ℃ through a heat exchanger 13, and the mixture is continuously conveyed to a hydrogenation and decoloration reactor 14. The hydrogen enters the catalyst bed layer together with the polymerization reaction liquid after being pressurized by the compressor, the reaction temperature in the hydrogenation and decoloration reactor 14 is controlled to be 240 ℃, the reaction pressure is controlled to be 6MPa,volume space velocity of 0.5h～1The hydrogen-oil ratio is 1000: 1.
The reaction liquid after the hydrogenation and the decoloration enters a second flash tank 15 for flash evaporation; the flash temperature in the second flash tank was controlled at 170 ℃ and the operating pressure at 80 kPa. Obtaining the inert solvent at the top of the second flash tank, and pumping the inert solvent to a polymerization solvent storage tank through a recovery pump for recycling of the polymerization reaction.
Obtaining hydrogenated resin liquid at the bottom of the second flash tank, and sending the hydrogenated resin liquid to a reduced pressure distillation tower 16 for continuously removing oligomers; controlling the tower top temperature of the distillation tower to be 220 ℃ and the operating pressure to be 20 kPa; discharging the oligomer from the top of the distillation tower, obtaining molten resin from the bottom of the distillation tower, and cooling to obtain solid light-colored dicyclopentadiene petroleum resin. The softening point was tested to be 107 ℃ and the Gardener colour was < 1.
Claims (5)
1. A method for continuously preparing light-colored dicyclopentadiene petroleum resin is characterized by comprising the following steps:
continuously feeding a dicyclopentadiene raw material and an inert solvent into a polymerization kettle for thermal polymerization, slowly heating to a polymerization temperature at the speed of 2-3 ℃/min, controlling the polymerization temperature in the polymerization kettle to be 220-270 ℃, the reaction pressure to be 0.5-2.0 MPa, the liquid level in the polymerization kettle to be 60-80%, and the retention time of materials at the polymerization temperature to be 0.5-20.0 h; obtaining a polymerization reaction liquid at an outlet of the polymerization kettle;
controlling the amount of the inert solvent in the reaction system in the polymerization kettle to be 55-85 wt% of the total amount of the reaction raw materials;
the inert solvent is at least one selected from aromatic hydrocarbon, naphthenic hydrocarbon, straight-chain alkane, dearomatized aliphatic hydrocarbon and isoparaffin;
conveying the obtained polymerization reaction liquid to a first flash tank for flash evaporation to remove unreacted monomers accounting for 0.5-4.0 wt% of the monomer raw materials, filtering out colloids and other impurities by using a 100-400-mesh filter screen filter, and then feeding the obtained polymerization reaction liquid into a hydrogenation reactor; controlling the reaction conditions of the hydrogenation reactor as follows: the reaction pressure is 6.0-15.0 MPa, the reaction temperature is 200-280 ℃, and the volume airspeed is 0.3-1.0 h～1The hydrogen-oil ratio is 500: 1-1000: 1; the hydrogenation catalyst is a supported palladium catalyst, and the mass of PdThe fraction is 0.5-2.0%, the catalyst carrier is gamma-Al 2O3, and the specific surface area is 80-250 m2/g；
The hydrogenated resin liquid obtained after hydrogenation is conveyed to a second flash tank to be evaporated to obtain a flash-evaporated resin liquid; controlling the flash evaporation temperature to be 170-200 ℃ and the flash evaporation pressure to be 80-200 kPa;
and (3) conveying the flash evaporation resin liquid to a distillation tower for reduced pressure distillation, controlling the temperature of the top of the distillation tower to be 180-220 ℃ and the operating pressure to be 10-20 kPa, discharging the oligomer from the top of the distillation tower, and obtaining the light-colored dicyclopentadiene petroleum resin at the bottom of the distillation tower.
2. The method for continuously preparing dicyclopentadiene petroleum resin with light color as claimed in claim 1, characterized in that the dicyclopentadiene raw material is petroleum cracking C5 mixture, and the dicyclopentadiene content in the dicyclopentadiene raw material is 67-87 wt%.
3. The method for continuously preparing dicyclopentadiene petroleum resin with a light color as claimed in claim 1, characterized in that the inert solvent is at least one selected from the group consisting of benzene, toluene, xylene, trimethylbenzene, hexane, cyclohexane, heptane, octane, nonane, decane, undecane, dodecane, mineral spirit No. 100, mineral spirit No. 200, solvent D40, solvent D60, Isopar H and Isopar L.
4. The method for continuously preparing dicyclopentadiene petroleum resin with light color as claimed in claim 1, wherein a gas phase outlet at the top of the polymerizer is sequentially connected with a condenser and a liquid separator, the gas phase substance in the polymerizer is introduced into the condenser through a pipeline to be condensed to 20-30 ℃, and then the separated liquid phase and the cyclopentadiene raw material enter a static mixer to be mixed and then enter the polymerizer from the lower part of the polymerizer.
5. The method for continuously preparing dicyclopentadiene petroleum resin with light color as claimed in claim 1, wherein the polymerization reaction liquid from the polymerization kettle is supplemented with inert solvent, mixed uniformly and then enters into the hydrogenation reactor; the amount of the added inert solvent is 0.5 to 5.0 wt% of the polymerization reaction liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810186351.4A CN108329429B (en) | 2018-03-07 | 2018-03-07 | Method for continuously preparing light-colored dicyclopentadiene petroleum resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810186351.4A CN108329429B (en) | 2018-03-07 | 2018-03-07 | Method for continuously preparing light-colored dicyclopentadiene petroleum resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108329429A CN108329429A (en) | 2018-07-27 |
| CN108329429B true CN108329429B (en) | 2020-08-21 |
Family
ID=62928958
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810186351.4A Active CN108329429B (en) | 2018-03-07 | 2018-03-07 | Method for continuously preparing light-colored dicyclopentadiene petroleum resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108329429B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716586B (en) * | 2022-04-22 | 2023-11-28 | 山东齐隆化工股份有限公司 | Process for producing hydrogenated resin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4604447A (en) * | 1983-11-22 | 1986-08-05 | Hercules Incorporated | Halogen-free, high flash point reactant solution |
| CN101555307A (en) * | 2009-05-09 | 2009-10-14 | 中国石油兰州石油化工公司 | Method for synthesizing poly-dicyclopentadiene petroleum resin with adjustable molecular weight, distribution and softening point |
| CN102558444A (en) * | 2010-12-17 | 2012-07-11 | 中国石油天然气股份有限公司 | Method for preparing dicyclopentadiene hydrogenated petroleum resin |
| CN203333552U (en) * | 2013-06-25 | 2013-12-11 | 朗盈科技（北京）有限公司 | Production system for synthesizing dicyclopentadiene petroleum resin |
| CN107252688A (en) * | 2017-05-15 | 2017-10-17 | 北京石油化工学院 | A kind of DCPD hydrogenation of petroleum resin catalyst and its preparation method and application |
-
2018
- 2018-03-07 CN CN201810186351.4A patent/CN108329429B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4604447A (en) * | 1983-11-22 | 1986-08-05 | Hercules Incorporated | Halogen-free, high flash point reactant solution |
| CN101555307A (en) * | 2009-05-09 | 2009-10-14 | 中国石油兰州石油化工公司 | Method for synthesizing poly-dicyclopentadiene petroleum resin with adjustable molecular weight, distribution and softening point |
| CN102558444A (en) * | 2010-12-17 | 2012-07-11 | 中国石油天然气股份有限公司 | Method for preparing dicyclopentadiene hydrogenated petroleum resin |
| CN203333552U (en) * | 2013-06-25 | 2013-12-11 | 朗盈科技（北京）有限公司 | Production system for synthesizing dicyclopentadiene petroleum resin |
| CN107252688A (en) * | 2017-05-15 | 2017-10-17 | 北京石油化工学院 | A kind of DCPD hydrogenation of petroleum resin catalyst and its preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108329429A (en) | 2018-07-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102382259B (en) | Industrial manufacture method for hydrogenated petroleum resin | |
| CN110372512B (en) | Separation and purification process of dimethyl carbonate | |
| CN108329429B (en) | Method for continuously preparing light-colored dicyclopentadiene petroleum resin | |
| US20140114102A1 (en) | Selective hydrogenation method for phenylacetylene in the presence of cracking c8 fraction | |
| CN105566032A (en) | Alkyne-rich C4 selective hydrogenation technology | |
| CN105585666A (en) | A preparing method of dicyclopentadiene hydrogenated petroleum resin | |
| CN101220124B (en) | Process for preparing decyclization C5 hydrogenation resin | |
| CN105646786A (en) | Method for preparing dicyclopentadiene hydrogenated petroleum resin from dicyclopentadiene directly | |
| CN103254038A (en) | Method for preparing cyclohexanol by using benzene | |
| CN100500719C (en) | Method for preparing petroleum resin by cracking C9 as raw material | |
| CN111574645B (en) | Hydrogenation method for high-sulfur petroleum resin | |
| CN102558444A (en) | Method for preparing dicyclopentadiene hydrogenated petroleum resin | |
| CN110003388B (en) | Preparation method of hydrogenated modified C5 petroleum resin | |
| CN116836067A (en) | Method for preparing diaminodiphenyl ether by continuous catalytic hydrogenation | |
| CN114436741B (en) | Preparation method of cyclopentene | |
| CN112479869B (en) | Method for rectifying dimethyl oxalate in coal chemical industry | |
| CN108299146B (en) | α -pinene isomerization reaction method | |
| CN102093511A (en) | Method for preparing dicyclopentadiene hydrogenated petroleum resin | |
| CN108059581B (en) | Method for preparing tetrahydronaphthalene by naphthalene hydrogenation | |
| CN108623476B (en) | Method for preparing amine products by hydrogenation of nitro compounds | |
| CN114805250B (en) | Tetrahydrofuran preparation process and device | |
| CN113264806B (en) | Method for preparing tetrahydronaphthalene, cis-decalin and trans-decalin by naphthalene hydrogenation | |
| CN210683648U (en) | Continuous polymerization system of C5/C9 copolymerized petroleum resin | |
| CN114621058B (en) | Preparation method of saturated cardanol by catalytic hydrogenation | |
| CN114425173B (en) | Device and method for recycling crude ethylene glycol in polyester production process |
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 |