CN105542080B - A kind of method that Petropols are prepared in microreactor - Google Patents
A kind of method that Petropols are prepared in microreactor Download PDFInfo
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- CN105542080B CN105542080B CN201511034516.9A CN201511034516A CN105542080B CN 105542080 B CN105542080 B CN 105542080B CN 201511034516 A CN201511034516 A CN 201511034516A CN 105542080 B CN105542080 B CN 105542080B
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- 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
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- 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
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of methods that Petropols are prepared in microreactor, it is desirable to provide a kind of heat that can be effectively conducted polymerization and generate early period prevents product from blocking the preparation methods of Petropols in the reactor because viscosity is excessive, and this method includes the following steps：1) the resin liquid fraction second that the resin liquid fraction first, boiling range that boiling range is 110 150 DEG C is 150 DEG C 190 DEG C is entered into micro- reaction channel with the flowing velocity of 2 20ml/h through single track micro-injection pump first, second；Solution third containing catalyst is entered into micro- reaction channel with the flowing velocity of 5 40ml/h through single track micro-injection pump third；At 40 130 DEG C, carries out one-step polymerization and react 2 10min；2) material is after the reaction of micro- reaction runner, into single screw extrusion machine, at 40 130 DEG C, carries out two sections of 3 5min of polymerisation；3) product is squeezed from outlet for product through single screw rod and is flowed out, and by alternately alkali cleaning, washing Removal of catalyst, flash distillation removing solvent, cooling pelletization obtains Petropols.
Description
Technical field
Invention is related to a kind of preparation method of Petropols, specifically, being to prepare Petropols in a kind of microreactor
Method.
Background technology
C9 Aromatic Petroleum Resins are a kind of thermoplastic resin of the C9 fractions through technique productions such as pre-treatment, polymerization, distillations.C9
Petropols have good water resistance, resistance to acid and alkali, weatherability and light fastness aging due to not polar functionalities in structure,
Dissolubility in organic solvent is good, good with the compatibility of other resins, also enbrittles, increasing stick, cohesiveness and plasticity.
It is mainly used for the fields such as coating, rubber chemicals, paper additive, ink and adhesive.In C9 fractions, phenylethylene, bicyclic penta
Dienes, indene resin are three kinds of main components that polymerisation occurs, and polymerisation early period occurs, and material aggregates into small molecule
Polymer, the process reaction is rapid, drastically heat release, be easy hot-spot, coloration deepens and coking, seriously affects product quality.
The middle and later periods is reacted, molecular weight polymers gradually increase, and polymerization rate is slow, heat release is greatly decreased, and viscosity increases, or even solid
Change.
Currently, there are mainly three types of Petropols polymerization process：Free radical polymerization synthesis technology, is urged at thermal polymerization process
Change polymerization synthesis technology.Free radical polymerization process makes C9 fractions occur to polymerize and is used by oxide causes free radical
Stop agent and stop polymerization, which does not use catalyst, so as to avoid the generation of waste water.Thermal polymerization advantage is not use to appoint
What catalyst and initiator, therefore waste water will not be generated.But above two polymerization synthesis technology has reaction temperature and pressure
The shortcomings of requirement of power is high, energy consumption is big, reaction rate is slow, coloured product is partially deep.Polymerization processes therewith reaction speed is fast, condition temperature
With production technology intermittently or serially, thus extensive use may be used.But C9 fractions are easy office in catalyzed polymerization process
Portion's buildup, when polymerization, discharge amount of heat, generate stain and coking, seriously limit range of reaction temperature with influence product at
Color and quality.Traditional reaction kettle can not solve the heat transfer problem of polymerisation early period, these problems limit the synthesis of product
Rate and quality.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of preparation method of Petropols, this method makes
Make monomer that catalytic polymerization occur with micro- reaction runner, the heat of polymerization generation early period can be effectively conducted, reuse single screw rod
Extruder makes molecular weight polymers continue that polymerisation occurs, and makes molecular weight polymers continue to grow up, uses Single screw extrusion C9
Petroleum resin products prevent product from being blocked in the reactor because viscosity is excessive.
In order to solve the above technical problems, first technical solution provided by the invention is as follows：
A kind of method that Petropols are prepared in microreactor includes following methods successively：
1) by cracking of ethylene by-product C9 double distilled lease making rectifying isolate boiling range be 110-150 DEG C resin liquid fraction first with
The flowing velocity of 2-20ml/h enters to micro- reaction channel through single track micro-injection pump first；By cracking of ethylene by-product C9 heavy distillat
Through rectifying isolate boiling range be 150 DEG C -190 DEG C of resin liquid fraction second with the flowing velocity of 2- 20ml/h through the micro note of single track
It penetrates pump second and enters to micro- reaction channel；By the solution third containing catalyst with the flowing velocity of 5-40ml/h through single track micro-injection pump
Third enters to micro- reaction channel；In 130 DEG C of 40-, carries out one-step polymerization and react 2-10min；
2) material is after the reaction of micro- reaction runner, and into single screw extrusion machine, at 40-130 DEG C, it is anti-to carry out two sections of polymerizations
Answer 3-5min；
3) product is squeezed from outlet for product through single screw rod and is flowed out, and by alternately alkali cleaning, washing Removal of catalyst, flash distillation is de-
Except solvent, cooling pelletization obtains Petropols.
Preferably, the method that Petropols are prepared in above-mentioned microreactor, the solution containing catalyst third are
BF3：AlCl3：The 0.1-2.0 in mass ratio of toluene：0.1-2.0：100 mix mixture.
Second technical solution provided by the invention is microreactor used when preparing Petropols, including micro- reaction stream
Road, described micro- reaction runner one end connect micro- reaction channel, and micro- reaction runner other end connects single screw extrusion machine；Micro- reaction is logical
Road connects three single track micro-injection pump first, single track micro-injection pump second disposed in parallel and single track micro-injection pump third.
Further, micro- reaction runner described in above-mentioned microreactor used when preparing Petropols is placed on constant temperature
In incubator, thermostatic protectiving incubator connects with cold cycling machine circuit.
Further, above-mentioned to prepare microreactor used when Petropols, micro- reaction stream Taoist priest 1-
15m, cross-sectional area 0.01-0.80mm2。
Further, above-mentioned to prepare microreactor used when Petropols, the spiral shell of the single screw extrusion machine
Shank diameter is 90-300mm.
Further, above-mentioned to prepare microreactor used when Petropols, micro- reaction stream Taoist priest 5m is horizontal
Sectional area is 0.50mm2。
Technical solution provided by the invention carries out C9 catalytic polymerizations using microreactor and produces Petropols, overcomes tradition
Reaction kettle reaction temperature cannot too high, hot-spot cause stain to generate and the shortcomings that coking.In one section of reaction, using miniature anti-
The feature for answering device heat conduction rapid so that the heat that C9 thermal polymerizations are largely released early period is timely conducted, and is accurately controlled anti-
The temperature for answering material obtains the polymerization small molecule of molecular weight uniform；In second-stage reaction, the Single screw extrusion of small cross-sectional area is used
Machine makes molecular weight polymers continue that polymerisation occurs, makes polymer continue to grow up, use single screw rod rotary extrusion C9 oil trees
Fat prod prevents highly viscous macromolecule polyalcohol from blocking, while can be accurately controlled temperature again, obtain molecular weight uniform and
Meet the C9 Petropols of the indexs such as softening point and coloration；The microreactor used substantially reduces space and energy needed for reaction
Consumption.
To sum up, there is technical solution provided by the invention reaction mass to be uniformly mixed, reaction rate is high, the residence time
It is short, reaction heat transfer it is rapid, polymer molecular weight is uniform, equipment investment is few, low energy consumption, can continuous production the advantages that, relatively
Previous technique can save production cost, reduce energy consumption.Since channel linear size is reduced to grade, microreactor it is whole
Body small volume, make operation is more controllable, safety is stronger, operation it is also more flexible.
Description of the drawings
Fig. 1 is microreactor structural schematic diagram provided by the invention.
Wherein：Micro- reaction runner 1, micro- reaction channel 2, single track micro-injection pump first 3a, single track micro-injection pump second 3b, list
The third 3c of road micro-injection pump, single screw extrusion machine 4, thermostatic protectiving incubator 5, cold-hot circulating machine 6.
Specific implementation mode
With reference to embodiment, the claim of the present invention is described in further detail, but do not constituted pair
Any restrictions of the present invention, anyone limited number of time made within the claims in the present invention protection domain modification, still in this hair
Within bright claims.
Embodiment 1
Microreactor provided by the invention, referring to Fig. 1, including micro- reaction runner 1, micro- reaction runner 1 is a length of
1-15m, cross-sectional area 0.01-0.80mm2, described micro- 1 one end of reaction runner connects micro- reaction channel 2, the company of micro- reaction channel 2
Three single track micro-injection pump first 3a disposed in parallel, single track micro-injection pump second 3b, single track micro-injection pump the third 3c are met, it is micro- anti-
1 other end of runner is answered to connect single screw extrusion machine 4；4 screw diameter of single screw extrusion machine is 90-300mm.
Micro- reaction runner 1 is arranged in wave, reduces floor space, increases the material reaction time, improves product
Yield.In order to facilitate heating, micro- reaction runner 1 is placed in thermostatic protectiving incubator 5, and the volume of thermostatic protectiving incubator 5 is micro-
React 1 volume of runner 1.3 times heat for convenience, and the heat-conducting medium is water or heat conduction industry oil；Thermostatic protectiving incubator
5 connect with 6 circuit of cold-hot circulating machine, are supplied to incubator heat.
Embodiment 2
The method that Petropols are prepared in a kind of microreactor provided by the invention, the micro- reaction provided using embodiment 1
Device, the specific method is as follows：
1) by cracking of ethylene by-product C9 double distilled lease making rectifying isolate boiling range be 130-150 DEG C resin liquid fraction first and
150 DEG C -170 DEG C of resin liquid fraction second is with the flowing velocity of 10ml/h, respectively through single track micro-injection pump first and micro note
It penetrates pump second and enters to micro- reaction channel 2；
2) solution third containing catalyst simultaneously, is entered into micro- reaction with the flowing velocity of 10ml/h through micro-injection pump third
Channel 2；The solution third is by BF3：AlCl3：In mass ratio the 0.5 of toluene:1.5:100 mix；
3) micro- reaction runner 1 is flowed into after micro- reaction channel 2 is sufficiently mixed, and catalytic polymerization 5min is carried out at 70 DEG C；
4) material is after the reaction of micro- reaction runner 1, and into single screw extrusion machine 4, two sections of polymerisations are carried out at 75 DEG C
3min；
5) product come out from single screw extrusion machine 4 passes through alternately 5%NaOH alkali cleanings, is washed to neutral Removal of catalyst,
Temperature is 210 DEG C of flash distillations, and removing solvent postcooling granulation, it is 80 DEG C to obtain softening point, the Petropols that coloration is 5.
Micro- reaction runner cross-sectional area is 0.5mm2, the long 5m of runner.The screw diameter of single screw extrusion machine is 90-
300mm。
Embodiment 3
The method that Petropols are prepared in a kind of microreactor provided by the invention, the micro- reaction provided using embodiment 1
Device, the specific method is as follows：
1) by cracking of ethylene by-product C9 double distilled lease making rectifying isolate boiling range be 130-150 DEG C resin liquid fraction first and
170 DEG C -190 DEG C of resin liquid fraction second is with the flowing velocity of 8ml/h, respectively through single track micro-injection pump first and micro-injection
Pump second enters to micro- reaction channel 2；
2) solution third containing catalyst simultaneously, is entered into micro- reaction with the flowing velocity of 15ml/h through micro-injection pump third
Channel 2；The solution third is by BF3：AlCl3：In mass ratio the 1 of toluene:1.5:100 mix；
3) micro- reaction runner 1 is flowed into after micro- reaction channel 2 is sufficiently mixed, and catalytic polymerization 10min is carried out at 90 DEG C；
4 materials are after the reaction of micro- reaction runner 1, and into single screw extrusion machine 4, two sections of polymerisations are carried out at 90 DEG C
3min；
5) product come out from single screw extrusion machine 4 passes through alternately 5%NaOH alkali cleanings, is washed to neutral Removal of catalyst,
Temperature is 210 DEG C of flash distillations, and removing solvent postcooling granulation, it is 80 DEG C to obtain softening point, the Petropols that coloration is 4.
Micro- reaction runner cross-sectional area is 0.5mm2, the long 5m of runner.The screw diameter of single screw extrusion machine is
150mm。
Embodiment 4
The method that Petropols are prepared in a kind of microreactor provided by the invention, the micro- reaction provided using embodiment 1
Device, the specific method is as follows：
1) by cracking of ethylene by-product C9 double distilled lease making rectifying isolate boiling range be 130-150 DEG C resin liquid fraction first with
The flowing velocity of 4ml/h, 170 DEG C -190 DEG C of resin liquid fraction second are micro through single track respectively with the flowing velocity of 16ml/h
Syringe pump first and micro-injection pump second enter to micro- reaction channel 2；
2) solution third containing catalyst simultaneously, is entered into micro- reaction with the flowing velocity of 10ml/h through micro-injection pump third
Channel 2；The solution third is by BF3：AlCl3：In mass ratio the 2 of toluene:2:100 mix；
3) micro- reaction runner 1 is flowed into after micro- reaction channel 2 is sufficiently mixed, and catalytic polymerization 5min is carried out at 110 DEG C；
4) material is after the reaction of micro- reaction runner 1, and into single screw extrusion machine 4, two sections of polymerisations are carried out at 100 DEG C
4min；
5) product come out from single screw extrusion machine 4 is flashed, and temperature is 210 DEG C, and removing solvent postcooling granulation obtains
It is 85 DEG C to softening point, the Petropols that coloration is 8
Micro- reaction runner cross-sectional area is 0.2mm2, the long 10m of runner.The screw diameter of single screw extrusion machine is
300mm。
Embodiment 5
The method that Petropols are prepared in a kind of microreactor provided by the invention, the micro- reaction provided using embodiment 1
Device, the specific method is as follows：
1) by cracking of ethylene by-product C9 double distilled lease making rectifying isolate boiling range be 110-130 DEG C resin liquid fraction first with
The flowing velocity of 14ml/h, 170 DEG C -190 DEG C of resin liquid fraction second are micro through single track respectively with the flowing velocity of 16ml/h
Syringe pump first and micro-injection pump second enter to micro- reaction channel 2；
2) solution third containing catalyst simultaneously, is entered into micro- reaction with the flowing velocity of 20ml/h through micro-injection pump third
Channel 2；The solution third is by BF3：AlCl3：In mass ratio the 1 of toluene:1:100 mix；
3) micro- reaction runner 1 is flowed into after micro- reaction channel 2 is sufficiently mixed, and catalytic polymerization 8min is carried out at 60 DEG C；
4) material is after the reaction of micro- reaction runner 1, and into single screw extrusion machine 4, two sections of polymerisations are carried out at 65 DEG C
3min；
5) product come out from single screw extrusion machine 4 is flashed, and temperature is 210 DEG C, and removing solvent postcooling granulation obtains
It is 120 DEG C to softening point, the Petropols that coloration is 10.
Micro- reaction runner cross-sectional area is 0.2mm2, the long 10m of runner；The screw diameter of single screw extrusion machine is
180mm。
Claims (6)
1. a kind of method for preparing Petropols in microreactor, which is characterized in that include following methods successively：
1) it is 110-150 DEG C of resin liquid fraction first with 2- boiling range to be isolated in cracking of ethylene by-product C9 double distilled lease making rectifying
The flowing velocity of 20ml/h enters to micro- reaction channel through single track micro-injection pump first；By cracking of ethylene by-product C9 double distilled lease makings
Rectifying isolates the resin liquid fraction second that boiling range is 150 DEG C -190 DEG C with the flowing velocity of 2-20ml/h through single track micro-injection pump
Second enters to micro- reaction channel；By the solution third containing catalyst with the flowing velocity of 5-40ml/h through single track micro-injection pump third into
Enter to micro- reaction channel；At 40-130 DEG C, carries out one-step polymerization and react 2-10min；
2) material is after the reaction of micro- reaction runner, into single screw extrusion machine, at 40-130 DEG C, carries out two sections of polymerisation 3-
5min；
3) product is squeezed from outlet for product through single screw rod and is flowed out, and by alternately alkali cleaning, washing Removal of catalyst, flash distillation removing is molten
Agent, cooling pelletization obtain Petropols；
The solution containing catalyst third described in step 1) is BF3：AlCl3：The 0.1-2.0 in mass ratio of toluene：0.1-2.0：100
Mix mixture.
2. described in claim 1 prepare microreactor used when Petropols, which is characterized in that including micro- reaction runner
(1), described micro- reaction runner (1) one end connects micro- reaction channel (2), and micro- reaction runner (1) other end connects Single screw extrusion
Machine (4)；Micro- reaction channel (2) connects three single track micro-injection pump first (3a) disposed in parallel, single track micro-injection pump second
(3b) and single track micro-injection pump third (3c).
3. according to claim 2 prepare microreactor used when Petropols, which is characterized in that micro- reaction
Runner (1) is placed in thermostatic protectiving incubator (5), and thermostatic protectiving incubator (5) connects with cold-hot circulating machine (6) circuit.
4. according to claim 2 prepare microreactor used when Petropols, which is characterized in that micro- reaction
Runner (1) long 1-15m, cross-sectional area 0.01-0.80mm2。
5. according to claim 4 prepare microreactor used when Petropols, which is characterized in that micro- reaction
Runner (1) long 5m, cross-sectional area 0.50mm2。
6. according to claim 2 prepare microreactor used when Petropols, which is characterized in that the single screw rod
The screw diameter of extruder (4) is 90-300mm.
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| CN201511034516.9A CN105542080B (en) | 2015-12-31 | 2015-12-31 | A kind of method that Petropols are prepared in microreactor |
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| CN105542080B true CN105542080B (en) | 2018-09-18 |
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| CN106478940B (en) * | 2016-11-01 | 2019-01-22 | 株洲时代新材料科技股份有限公司 | Prepare continuous micro-reaction device, method and the product of meta-aramid resin |
| CN106674404B (en) * | 2016-12-29 | 2019-04-19 | 彤程化学（中国）有限公司 | A method of utilizing molecular distillation technique continuous production hydrocarbon resin |
| CN110229329A (en) * | 2019-05-13 | 2019-09-13 | 中国科学技术大学 | A kind of biomass-based furans polyamide continuous production device of high polymerization degree half and continuous producing method |
| CN112851858B (en) * | 2021-01-13 | 2022-09-16 | 淄博鲁华泓锦新材料集团股份有限公司 | C5 petroleum resin takes off system of urging |
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|---|---|---|---|---|
| CN102702434A (en) * | 2012-06-07 | 2012-10-03 | 抚顺齐隆化工有限公司 | Method of two-stage continuous polymerization production of petroleum resin |
| CN102807631A (en) * | 2012-08-15 | 2012-12-05 | 罗吉尔 | Pipeline-type continuous polymerization reaction method |
| CN104045770A (en) * | 2013-03-13 | 2014-09-17 | 中国石油化工股份有限公司 | Preparation method of C9 petroleum resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005152727A (en) * | 2003-11-21 | 2005-06-16 | Suehiro Epm:Kk | Extruder type continuous reactor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702434A (en) * | 2012-06-07 | 2012-10-03 | 抚顺齐隆化工有限公司 | Method of two-stage continuous polymerization production of petroleum resin |
| CN102807631A (en) * | 2012-08-15 | 2012-12-05 | 罗吉尔 | Pipeline-type continuous polymerization reaction method |
| CN104045770A (en) * | 2013-03-13 | 2014-09-17 | 中国石油化工股份有限公司 | Preparation method of C9 petroleum resin |
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