CN106893034A - A kind of ethene m-pentadiene petro-resin and preparation method - Google Patents
A kind of ethene m-pentadiene petro-resin and preparation method Download PDFInfo
- Publication number
- CN106893034A CN106893034A CN201710206073.XA CN201710206073A CN106893034A CN 106893034 A CN106893034 A CN 106893034A CN 201710206073 A CN201710206073 A CN 201710206073A CN 106893034 A CN106893034 A CN 106893034A
- Authority
- CN
- China
- Prior art keywords
- pentadiene
- ethene
- parts
- reactor
- petro
- 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.)
- Pending
Links
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
- C08F236/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F236/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F236/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F236/08—Isoprene
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of ethene m-pentadiene petro-resin and preparation method, including the following raw material：Pentadiene concentrate, vinyl monomer, catalyst, toluene, age resistor, alkali lye, demulsifier, also including appropriate water.Preparation method includes：First to a small amount of toluene and anhydrous Aluminum chloride is added in reactor, residual toluene is added while stirring, then protected to logical nitrogen in reactor；Pentadiene concentrate and vinyl monomer are weighed according to proportioning, is slowly dropped in reactor, control temperature for 40 ~ 60 DEG C after completion of dropwise addition, react 5 ~ 7h；Alkali lye, demulsifier and suitable quantity of water are added, 30 ~ 40min is stirred, a point liquid is stood, supernatant liquid is taken, purified, that is, obtain described ethene m-pentadiene petro-resin.Petropols of the present invention not only have softening point higher, also substantially increase melt viscosity, range of application and the field of Petropols are expanded, with preferable application value.
Description
Technical field
The present invention relates to Petropols technical field, and in particular to a kind of ethene-m-pentadiene petro-resin and preparation side
Method.
Background technology
Petropols are that, with the C5 of cracking of ethylene byproduct in process, C9 cuts are a kind of thermoplastic of main polymerizable raw material
Property resin.C5 series Petropols are that, by petroleum cracking byproduct, light dydrocarbon series Petropols are widely used, wherein pentadiene
Petropols can be used to manufacture contact adhesive, PUR flux, hot-melt coating encapsulating material, hot melt traffic sign coating, rubber
Glue tackifier, paint and varnish, printing-ink etc..The m-pentadiene petro-resin product of prior art production, its softening point one
As below 105 DEG C, melt viscosity then in 300cps (200 DEG C, together later) below.However, in some special application scenarios,
In the adhesive used in traffic paint, hot environment that such as torrid areas uses, often require that this kind of Petropols have higher
Softening point and melt viscosity, for example, softening point requirement is more than 110 DEG C, melt viscosity is preferably in more than 500cps.
Therefore, a kind of softening point that can either improve Petropols, and the oil tree with melt viscosity higher are researched and developed
Fat and its synthetic method turn into the emphasis of research at present, it may have preferable application prospect and use value.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of ethene-m-pentadiene petro-resin and system
Preparation Method, the Petropols not only have softening point higher, also substantially increase melt viscosity, expand Petropols
Range of application and field, with preferable application value.Additionally, the preparation method is simple and easy to apply, it is adapted to popularization and application.
The present invention solves technical problem and adopts the following technical scheme that：
The present invention relates to a kind of ethene-m-pentadiene petro-resin, including following weight portion each raw material：Pentadiene concentrate
60 ~ 90 parts, 10 ~ 20 parts of vinyl monomer, 0.1 ~ 5 part of catalyst, 80 ~ 150 parts of toluene, 0.6 ~ 1.5 part of age resistor, alkali lye 0.1 ~ 3
Part, 0.5 ~ 5 part of demulsifier, also including appropriate water.
Preferably, 80 parts of the pentadiene concentrate, 15 parts of vinyl monomer, 0.68 part of catalyst, 120 parts of toluene, anti-
1.1 parts of old agent, 0.6 part of alkali lye, 2.5 parts of demulsifier, also including appropriate water.
Preferably, the pentadiene concentrate is that pentadiene weight/mass percentage composition is more than 85%, isoprene and ring penta
Mixture of the diene weight/mass percentage composition less than 5%.
Preferably, the catalyst is AlCl3。
Preferably, the age resistor is phenol antiager.
The invention further relates to a kind of method for preparing ethene-m-pentadiene petro-resin, comprise the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, first to adding a small amount of toluene and anhydrous chlorination in reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and is then protected to logical nitrogen in reactor；
（2）Weigh pentadiene concentrate and vinyl monomer according to proportioning, be slowly dropped in reactor, control dropping temperature and
Rate of addition, controls temperature for 40 ~ 60 DEG C after completion of dropwise addition, react 5 ~ 7h；
（3）To alkali lye, demulsifier and suitable quantity of water is added in reacted mixture, 30 ~ 40min is stirred in 40 ~ 60 DEG C, stand and divide
Liquid, takes supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity are removed, that is, is obtained described ethene-penta 2
Alkene Petropols.
Preferably, the step（2）The temperature that reactor is also first adjusted before middle dropwise reaction monomer is 0 ~ 10 DEG C.
Preferably, the step（2）The feed postition of middle pentadiene concentrate and vinyl monomer is to be respectively placed in dropping liquid
In funnel, while being added dropwise in reactor, rate of addition is controlled so that reaction monomers are in 20 ~ 30min completion of dropping.
Preferably, the step（4）Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Compared with prior art, the present invention has following beneficial effect：
（1）Ethene-m-pentadiene petro-resin of the present invention, by by ethene and pentadiene concentrate combined polymerization, making
Obtaining the Petropols not only has softening point higher, also substantially increases melt viscosity；Due to the presence of monoolefine so that
Petropols have preferable dissolubility, range of application and the field of Petropols are expanded, with preferable application value.
（2）The preparation process is simple of ethene-m-pentadiene petro-resin of the present invention, reaction condition is gentle, operation
It is convenient, due to the inventory of the inventory more than ethene of pentadiene so that have certain molecule inner injection in process of production
Close, improve the stability of product, the solid matter for preventing intermolecular cross-linking from producing increases unnecessary processing step.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, generally according to normal condition, for example
Sambrook equimoleculars are cloned：Laboratory manual（New York:Cold Spring Harbor Laboratory Press,
1989）Described in condition, or according to the condition proposed by manufacturer.
Embodiment 1：
A kind of ethene-m-pentadiene petro-resin and preparation method of the preferred embodiment of the present invention；
Ethene-the m-pentadiene petro-resin, is prepared from by each raw material of following parts by weight：
80 parts of pentadiene concentrate；
15 parts of vinyl monomer；
0.68 part of catalyst；
120 parts of toluene；
1.1 parts of age resistor；
0.6 part of alkali lye；
2.5 parts of demulsifier；
Also include appropriate water.
The pentadiene concentrate is that pentadiene weight/mass percentage composition is 90%, isoprene and cyclopentadiene quality
Mixture of the percentage composition less than 10%.
The catalyst is AlCl3。
The age resistor is phenol antiager.
The method for preparing ethene-m-pentadiene petro-resin of the present invention, comprises the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, first to adding a small amount of toluene and anhydrous chlorination in reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and is then protected to logical nitrogen in reactor；
（2）Weigh pentadiene concentrate and vinyl monomer according to proportioning, be slowly dropped in reactor, control dropping temperature and
Rate of addition, controls temperature for 50 DEG C after completion of dropwise addition, react 6h；
（3）To alkali lye, demulsifier and suitable quantity of water is added in reacted mixture, 30min is stirred in 50 DEG C, stand a point liquid, taken
Supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity are removed, that is, is obtained described ethene-penta 2
Alkene Petropols.
Step（2）The temperature that reactor is also first adjusted before middle dropwise reaction monomer is 5 ~ 8 DEG C.
Step（2）The feed postition of middle pentadiene concentrate and vinyl monomer is to be respectively placed in dropping funel, while
It is added dropwise in reactor, controls rate of addition so that reaction monomers are in 30min completion of dropping.
Step（4）Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Ethene-m-pentadiene petro-resin that the present embodiment is prepared is according to GB 4507 ~ 1999《Asphalt softening point is surveyed
Determine method》, and the melt viscosity of modified resin is detected at 200 DEG C by Bu Shi rotary viscometers, it is as a result as follows：
Softening point is 131 DEG C, melt viscosity 650cps.
Embodiment 2：
A kind of ethene-m-pentadiene petro-resin and preparation method of the preferred embodiment of the present invention；
Ethene-the m-pentadiene petro-resin, is prepared from by each raw material of following parts by weight：
60 parts of pentadiene concentrate；
10 parts of vinyl monomer；
0.1 part of catalyst；
80 parts of toluene；
0.6 part of age resistor；
0.1 part of alkali lye；
0.5 part of demulsifier；
Also include appropriate water.
The pentadiene concentrate is that pentadiene weight/mass percentage composition is 85%, isoprene and cyclopentadiene quality
Mixture of the percentage composition less than 15%.
The catalyst is AlCl3。
The age resistor is phenol antiager.
The method for preparing ethene-m-pentadiene petro-resin of the present invention, comprises the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, first to adding a small amount of toluene and anhydrous chlorination in reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and is then protected to logical nitrogen in reactor；
（2）Weigh pentadiene concentrate and vinyl monomer according to proportioning, be slowly dropped in reactor, control dropping temperature and
Rate of addition, controls temperature for 40 DEG C after completion of dropwise addition, react 7h；
（3）To alkali lye, demulsifier and suitable quantity of water is added in reacted mixture, 40min is stirred in 40 DEG C, stand a point liquid, taken
Supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity are removed, that is, is obtained described ethene-penta 2
Alkene Petropols.
Step（2）The temperature that reactor is also first adjusted before middle dropwise reaction monomer is 0 ~ 5 DEG C.
Step（2）The feed postition of middle pentadiene concentrate and vinyl monomer is to be respectively placed in dropping funel, while
It is added dropwise in reactor, controls rate of addition so that reaction monomers are in 20min completion of dropping.
Step（4）Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Ethene-m-pentadiene petro-resin that the present embodiment is prepared is according to GB 4507 ~ 1999《Asphalt softening point is surveyed
Determine method》, and the melt viscosity of modified resin is detected at 200 DEG C by Bu Shi rotary viscometers, it is as a result as follows：
Softening point is 119 DEG C, melt viscosity 602cps.
Embodiment 3：
A kind of ethene-m-pentadiene petro-resin and preparation method of the preferred embodiment of the present invention；
Ethene-the m-pentadiene petro-resin, is prepared from by each raw material of following parts by weight：
90 parts of pentadiene concentrate；
20 parts of vinyl monomer；
5 parts of catalyst；
150 parts of toluene；
1.5 parts of age resistor；
3 parts of alkali lye；
5 parts of demulsifier；
Also include appropriate water.
The pentadiene concentrate is that pentadiene weight/mass percentage composition is 88%, isoprene and cyclopentadiene quality
Mixture of the percentage composition less than 12%.
The catalyst is AlCl3。
The age resistor is phenol antiager.
The method for preparing ethene-m-pentadiene petro-resin of the present invention, comprises the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, first to adding a small amount of toluene and anhydrous chlorination in reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and is then protected to logical nitrogen in reactor；
（2）Weigh pentadiene concentrate and vinyl monomer according to proportioning, be slowly dropped in reactor, control dropping temperature and
Rate of addition, controls temperature for 60 DEG C after completion of dropwise addition, react 5h；
（3）To alkali lye, demulsifier and suitable quantity of water is added in reacted mixture, 30min is stirred in 60 DEG C, stand a point liquid, taken
Supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity are removed, that is, is obtained described ethene-penta 2
Alkene Petropols.
Step（2）The temperature that reactor is also first adjusted before middle dropwise reaction monomer is 8 ~ 10 DEG C.
Step（2）The feed postition of middle pentadiene concentrate and vinyl monomer is to be respectively placed in dropping funel, while
It is added dropwise in reactor, controls rate of addition so that reaction monomers are in 30min completion of dropping.
Step（4）Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Ethene-m-pentadiene petro-resin that the present embodiment is prepared is according to GB 4507 ~ 1999《Asphalt softening point is surveyed
Determine method》, and the melt viscosity of modified resin is detected at 200 DEG C by Bu Shi rotary viscometers, it is as a result as follows：
Softening point is 126 DEG C, melt viscosity 633cps.
Ethene-m-pentadiene petro-resin of the present invention, by by ethene and pentadiene concentrate combined polymerization, making
Obtaining the Petropols not only has softening point higher, also substantially increases melt viscosity；Due to the presence of monoolefine so that
Petropols have preferable dissolubility, range of application and the field of Petropols are expanded, with preferable application value.
The preparation process is simple of ethene-m-pentadiene petro-resin of the present invention, reaction condition is gentle, operation side
Just so that have certain intramolecular polymerization in process of production, improve the stability of product, prevent intermolecular cross-linking from producing
Solid matter, increase unnecessary processing step.
Specific embodiment of the invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can within the scope of the claims make various deformations or amendments, this not shadow
Sound substance of the invention.
Claims (9)
1. a kind of ethene-m-pentadiene petro-resin, it is characterised in that：Each raw material including following weight portion：Pentadiene is dense
60 ~ 90 parts of contracting thing, 10 ~ 20 parts of vinyl monomer, 0.1 ~ 5 part of catalyst, 80 ~ 150 parts of toluene, 0.6 ~ 1.5 part of age resistor, alkali lye
0.1 ~ 3 part, 0.5 ~ 5 part of demulsifier, also including appropriate water.
2. ethene-m-pentadiene petro-resin according to claim 1, it is characterised in that：The pentadiene concentrate
80 parts, 15 parts of vinyl monomer, 0.68 part of catalyst, 120 parts of toluene, 1.1 parts of age resistor, 0.6 part of alkali lye, 2.5 parts of demulsifier, also
Including appropriate water.
3. ethene-m-pentadiene petro-resin according to claim 1, it is characterised in that：The pentadiene concentrate
For pentadiene weight/mass percentage composition is more than 85%, the mixture of isoprene and cyclopentadiene weight/mass percentage composition less than 5%.
4. ethene-m-pentadiene petro-resin according to claim 1, it is characterised in that：The catalyst is AlCl3。
5. ethene-m-pentadiene petro-resin according to claim 1, it is characterised in that：The age resistor is anti-for phenols
Old agent.
6. the method that one kind prepares the ethene-m-pentadiene petro-resin as described in any one of claim 1 ~ 5, its feature exists
In：Comprise the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, first to adding a small amount of toluene and anhydrous chlorination in reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and is then protected to logical nitrogen in reactor；
（2）Weigh pentadiene concentrate and vinyl monomer according to proportioning, be slowly dropped in reactor, control dropping temperature and
Rate of addition, controls temperature for 40 ~ 60 DEG C after completion of dropwise addition, react 5 ~ 7h；
（3）To alkali lye, demulsifier and suitable quantity of water is added in reacted mixture, 30 ~ 40min is stirred in 40 ~ 60 DEG C, stand and divide
Liquid, takes supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity are removed, that is, is obtained described ethene-penta 2
Alkene Petropols.
7. the preparation method of ethene-m-pentadiene petro-resin according to claim 6, it is characterised in that：The step
（2）The temperature that reactor is also first adjusted before middle dropwise reaction monomer is 0 ~ 10 DEG C.
8. the preparation method of ethene-m-pentadiene petro-resin according to claim 6, it is characterised in that：The step
（2）The feed postition of middle pentadiene concentrate and vinyl monomer is to be respectively placed in dropping funel, while being dripped in reactor
Plus, control rate of addition so that reaction monomers are in 20 ~ 30min completion of dropping.
9. the preparation method of ethene-m-pentadiene petro-resin according to claim 6, it is characterised in that：The step
（4）Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710206073.XA CN106893034A (en) | 2017-03-31 | 2017-03-31 | A kind of ethene m-pentadiene petro-resin and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710206073.XA CN106893034A (en) | 2017-03-31 | 2017-03-31 | A kind of ethene m-pentadiene petro-resin and preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106893034A true CN106893034A (en) | 2017-06-27 |
Family
ID=59193451
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710206073.XA Pending CN106893034A (en) | 2017-03-31 | 2017-03-31 | A kind of ethene m-pentadiene petro-resin and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106893034A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1448417A (en) * | 2002-04-04 | 2003-10-15 | 中国石化上海石油化工股份有限公司 | Prep. of high softening point and high fusion viscosity pentadiene petroleum resin |
| CN103214622A (en) * | 2012-01-18 | 2013-07-24 | 中国石油天然气股份有限公司 | Method for improving softening point of 1,3-pentadiene petroleum resin |
| CN104448141A (en) * | 2013-09-22 | 2015-03-25 | 梁懿 | M-pentadiene petroleum resin synthesis technology |
| CN106317758A (en) * | 2016-08-31 | 2017-01-11 | 广西交通科学研究院 | Special colored asphalt cementing agent for water drainage pavement and preparation method of special colored asphalt cementing agent |
-
2017
- 2017-03-31 CN CN201710206073.XA patent/CN106893034A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1448417A (en) * | 2002-04-04 | 2003-10-15 | 中国石化上海石油化工股份有限公司 | Prep. of high softening point and high fusion viscosity pentadiene petroleum resin |
| CN103214622A (en) * | 2012-01-18 | 2013-07-24 | 中国石油天然气股份有限公司 | Method for improving softening point of 1,3-pentadiene petroleum resin |
| CN104448141A (en) * | 2013-09-22 | 2015-03-25 | 梁懿 | M-pentadiene petroleum resin synthesis technology |
| CN106317758A (en) * | 2016-08-31 | 2017-01-11 | 广西交通科学研究院 | Special colored asphalt cementing agent for water drainage pavement and preparation method of special colored asphalt cementing agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US2338741A (en) | Substituted styrene-polybutadiene copolymer | |
| CN106916264B (en) | A kind of C5 Petropols and its synthetic method that aromatic hydrocarbon is modified | |
| CN102718927A (en) | Production method for coumarone resin | |
| CN102643389A (en) | Preparation method for petroleum resin with high softening point | |
| US2317859A (en) | Styrene-polypiperylene copolymer | |
| CN105348443B (en) | The preparation method of synthesizing pentadiene Petropols catalyst system and catalyzing and m-pentadiene petro-resin | |
| CN107778389B (en) | Synthesis method of styrene modified dicyclopentadiene hydrogenated resin | |
| CN106893034A (en) | A kind of ethene m-pentadiene petro-resin and preparation method | |
| US2894937A (en) | Process for preparing petroleum resins ii | |
| KR100191475B1 (en) | Blanched block copolymer, process for its preparation and use therefor | |
| JPS6195013A (en) | Petroleum resin and its production | |
| CN106893056B (en) | A kind of modified dicyclopentadiene petroleum resin of s-B-S and preparation method | |
| CN105764937A (en) | Functional polyisobutylene-containing oligomers and polymers | |
| EP0057510B1 (en) | Improvements in the production of hydrocarbon resins and products resulting therefrom | |
| CN104072666B (en) | Preparation method of liquid m-pentadiene petroleum resin | |
| CN103102449A (en) | Manufacturing method of piperylene petroleum resin | |
| US4403080A (en) | Isomerization and polymerization of hydrocarbon resins | |
| CN103881027B (en) | The synthetic method of m-pentadiene petro-resin | |
| US2338742A (en) | Substituted styrene-polyisoprene copolymer | |
| US3880820A (en) | Method for producing thermoplastic resin | |
| CN106699972B (en) | A kind of preparation method and its device of C5/C10 copolymer resins | |
| US2862982A (en) | Removal of alkali metals from viscous hydrocarbon liquids | |
| CN106947024A (en) | C5 Petropols and preparation method that a kind of iso-amylene is modified | |
| JPH0221403B2 (en) | ||
| US2562090A (en) | Polymerization of dibromobutene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170627 |
|
| RJ01 | Rejection of invention patent application after publication |