CN106947024A - C5 Petropols and preparation method that a kind of iso-amylene is modified - Google Patents
C5 Petropols and preparation method that a kind of iso-amylene is modified Download PDFInfo
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- CN106947024A CN106947024A CN201710206159.2A CN201710206159A CN106947024A CN 106947024 A CN106947024 A CN 106947024A CN 201710206159 A CN201710206159 A CN 201710206159A CN 106947024 A CN106947024 A CN 106947024A
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- amylene
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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
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/14—Monomers containing five or more carbon atoms
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D157/00—Coating compositions based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The C5 Petropols and preparation method being modified the invention discloses a kind of iso-amylene, including the following raw material：Iso-amylene, C 5 fraction, catalyst, toluene, age resistor, alkali lye, demulsifier, also including appropriate water.Preparation method includes：A small amount of toluene and anhydrous Aluminum chloride is first added into reactor, residual toluene is added while stirring, nitrogen protection is then led into reactor；C 5 fraction and isoamyl alkene monomer are weighed according to proportioning, is slowly dropped in reactor, it is 40 ~ 60 DEG C that temperature is controlled after completion of dropwise addition, reacts 5 ~ 7.5h；Alkali lye, demulsifier and suitable quantity of water are added into reacted mixture, 30 ~ 50min is stirred in 40 ~ 60 DEG C, a point liquid is stood, takes supernatant liquid；Purification produces the C5 Petropols of iso-amylene modification.Petropols lighter color of the present invention, softening point is high, has preferable stability applied to traffic paint, with preferable application value.
Description
Technical field
The present invention relates to Petropols technical field, and in particular to C5 Petropols and preparation side that a kind of iso-amylene is modified
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, available for manufacture pressure
Sensitive adhesive, PUR flux, hot-melt coating encapsulating material, hot melt traffic sign coating, rubber tackifier, paint and varnish,
Printing-ink etc..
C5 Petropols are mainly used in the fields such as traffic paint, pressure sensitive adhesive, tire, ink.Its production of the resin of different purposes
Raw material is also different.Cyclopentadiene and dicyclopentadiene in C 5 fraction, its activity are very strong, in aluminum trichloride catalyst
Under, polymerisation is very violent, and reaction is whard to control, easily generates gel.The resin color and luster of generation, softening point, are melted viscous simultaneously
The indexs such as degree are all poor.So requiring that the total amount of cyclopentadiene and dicyclopentadiene is less than 2% in general resin raw material.Together
When the excessive crosslinking of C5 Petropols is caused due to the isoprene content Gao Shihui in resin raw material, make the dissolving of resin
Property, compatibility be deteriorated, molecular weight be not easy to control, its color and luster, softening point are difficult the use requirement for meeting traffic paint.Pressure sensitive adhesive etc.
Adhesive industry requires that the content of isoprene in resin raw material is less than 3%.And traffic paint with C5 Petropols in raw material
Isoprene just without so strict, but still to have controlled.
The content of the invention
For defect of the prior art, the C5 Petropols being modified it is an object of the invention to provide a kind of iso-amylene and system
Preparation Method, the Petropols lighter color, softening point is high, has preferable stability applied to traffic paint, is answered with preferable
With value.
The present invention solves technical problem and adopted the following technical scheme that：
The present invention relates to the C5 Petropols that a kind of iso-amylene is modified, include each raw material of following parts by weight：Iso-amylene 20 ~ 36
Part, 60 ~ 85 parts of C 5 fraction, 0.1 ~ 3 part of catalyst, 80 ~ 150 parts of toluene, 0.8 ~ 1.6 part of age resistor, 0.5 ~ 2 part of alkali lye, demulsification
0.5 ~ 4.6 part of agent, also including appropriate water.
Preferably, 32 parts of the iso-amylene, 78 parts of C 5 fraction, 1.2 parts of catalyst, 120 parts of toluene, 1.4 parts of age resistor, alkali
0.9 part of liquid, 3.3 parts of demulsifier, also including appropriate water.
Preferably, the C 5 fraction including the content of quality hundred be respectively isoprene 35% ~ 55%, pentadiene 20% ~ 40%,
Cyclopentadiene 5% ~ 10%, remaining component is less than 0.1%.
Preferably, the catalyst is AlCl3。
Preferably, the age resistor is phenol antiager.
The invention further relates to a kind of method for the C5 Petropols for preparing iso-amylene modification, comprise the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, and a small amount of toluene and anhydrous chlorination are first added into reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and nitrogen protection is then led into reactor；
（2）C 5 fraction and isoamyl alkene monomer are weighed according to proportioning, is slowly dropped in reactor, control dropping temperature and dropwise addition speed
Degree, it is 40 ~ 60 DEG C that temperature is controlled after completion of dropwise addition, reacts 5 ~ 7.5h；
（3）Alkali lye, demulsifier and suitable quantity of water are added into reacted mixture, 30 ~ 50min is stirred in 40 ~ 60 DEG C, stands and divides
Liquid, takes supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity is removed, that is, obtains what described iso-amylene was modified
C5 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 C 5 fraction and isoamyl alkene monomer is：Respectively by C 5 fraction and isoamyl
Alkene monomer is placed in two dropping funels, while being added dropwise into reactor, controls rate of addition so that reaction monomers 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）The C5 Petropols that iso-amylene of the present invention is modified, by by the alkadienes copolymerization in iso-amylene and C 5 fraction
Close so that the Petropols lighter color of preparation, softening point are high, when being applied to making highway sign, graticule traffic paint, with road
Face has a higher bond strength, and with wearability is high, resistance to sunshine-duration length, the features such as antioxygenic property is good, greatly increase
The service life of traffic paint, reduces use cost, with preferable application value and prospect.
（2）The preparation technology for the C5 Petropols that iso-amylene of the present invention is modified is simple, and reaction condition is gentle, operation
Convenient, production equipment and power consumption are less, reduce production difficulty and production cost, are adapted to popularization and application.
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 method 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：
C5 Petropols and preparation method that a kind of iso-amylene of the preferred embodiment of the present invention is modified；
The C5 Petropols that the iso-amylene is modified, are prepared from by each raw material of following parts by weight：
32 parts of iso-amylene；
78 parts of C 5 fraction；
1.2 parts of catalyst；
120 parts of toluene；
1.4 parts of age resistor；
0.9 part of alkali lye；
3.3 parts of demulsifier；
Also include appropriate water.
The C 5 fraction is respectively isoprene 35% ~ 55%, pentadiene 20% ~ 40%, ring penta 2 including the content of quality hundred
Alkene 5% ~ 10%, remaining component is less than 0.1%.
The catalyst is AlCl3。
The age resistor is phenol antiager.
The method of the C5 Petropols of the present invention for preparing iso-amylene modification, comprises the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, and a small amount of toluene and anhydrous chlorination are first added into reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and nitrogen protection is then led into reactor；
（2）C 5 fraction and isoamyl alkene monomer are weighed according to proportioning, is slowly dropped in reactor, control dropping temperature and dropwise addition speed
Degree, it is 50 DEG C that temperature is controlled after completion of dropwise addition, reacts 6h；
（3）Alkali lye, demulsifier and suitable quantity of water are added into reacted mixture, 40min is stirred in 50 DEG C, a point liquid is stood, takes
Supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity is removed, that is, obtains what described iso-amylene was modified
C5 Petropols.
Step（2）The temperature that reactor is also first adjusted before middle dropwise reaction monomer is 5 ~ 7 DEG C.
Step（2）The feed postition of middle C 5 fraction and isoamyl alkene monomer is：C 5 fraction and isoamyl alkene monomer are placed in respectively
In two dropping funels, while being added dropwise into reactor, rate of addition is controlled 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.
The C5 Petropols that the iso-amylene that the present embodiment is prepared is modified are respectively according to GB 4507 ~ 1999《Pitch softens
Point determination method》、GBT22295~2008《Transparency liquid colourity is monitored》The softening point and colourity of modified petroleum resin are examined
Survey, 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
For 122 DEG C, colourity 4, melt viscosity 160cps.
Embodiment 2：
C5 Petropols and preparation method that a kind of iso-amylene of the preferred embodiment of the present invention is modified；
The C5 Petropols that the iso-amylene is modified, are prepared from by each raw material of following parts by weight：
20 parts of iso-amylene；
60 parts of C 5 fraction；
0.1 part of catalyst；
80 parts of toluene；
0.8 part of age resistor；
0.5 part of alkali lye；
0.5 part of demulsifier；
Also include appropriate water.
The C 5 fraction is respectively isoprene 55%, pentadiene 35%, cyclopentadiene 10% including the content of quality hundred, its
Remaining component is less than 0.1%.
The catalyst is AlCl3。
The age resistor is phenol antiager.
The method of the C5 Petropols of the present invention for preparing iso-amylene modification, comprises the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, and a small amount of toluene and anhydrous chlorination are first added into reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and nitrogen protection is then led into reactor；
（2）C 5 fraction and isoamyl alkene monomer are weighed according to proportioning, is slowly dropped in reactor, control dropping temperature and dropwise addition speed
Degree, it is 40 DEG C that temperature is controlled after completion of dropwise addition, reacts 7.5h；
（3）Alkali lye, demulsifier and suitable quantity of water are added into reacted mixture, 30min is stirred in 40 ~ 60 DEG C, a point liquid is stood,
Take supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity is removed, that is, obtains what described iso-amylene was modified
C5 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 C 5 fraction and isoamyl alkene monomer is：C 5 fraction and isoamyl alkene monomer are placed in respectively
In two dropping funels, while being added dropwise into reactor, rate of addition is controlled 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.
The modification dicyclopentadiene petroleum resin that the present embodiment is prepared is respectively according to GB 4507 ~ 1999《Pitch softens
Point determination method》、GBT22295~2008《Transparency liquid colourity is monitored》The softening point and colourity of modified petroleum resin are examined
Survey, 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
For 118 DEG C, colourity 4, melt viscosity 140cps.
Embodiment 3：
C5 Petropols and preparation method that a kind of iso-amylene of the preferred embodiment of the present invention is modified；
The C5 Petropols that the iso-amylene is modified, are prepared from by each raw material of following parts by weight：
36 parts of iso-amylene；
85 parts of C 5 fraction；
3 parts of catalyst；
150 parts of toluene；
1.6 parts of age resistor；
2 parts of alkali lye；
4.6 parts of demulsifier；
Also include appropriate water.
Preferably, 32 parts of the iso-amylene, 78 parts of C 5 fraction, 1.2 parts of catalyst, 120 parts of toluene, 1.4 parts of age resistor, alkali
0.9 part of liquid, 3.3 parts of demulsifier, also including appropriate water.
The C 5 fraction is respectively isoprene 55%, pentadiene 40%, cyclopentadiene 5% including the content of quality hundred, remaining
Component is less than 0.1%.
The catalyst is AlCl3。
The age resistor is phenol antiager.
The method of the C5 Petropols of the present invention for preparing iso-amylene modification, comprises the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, and a small amount of toluene and anhydrous chlorination are first added into reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and nitrogen protection is then led into reactor；
（2）C 5 fraction and isoamyl alkene monomer are weighed according to proportioning, is slowly dropped in reactor, control dropping temperature and dropwise addition speed
Degree, it is 60 DEG C that temperature is controlled after completion of dropwise addition, reacts 5h；
（3）Alkali lye, demulsifier and suitable quantity of water are added into reacted mixture, 30min is stirred in 60 DEG C, a point liquid is stood, takes
Supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity is removed, that is, obtains what described iso-amylene was modified
C5 Petropols.
Step（2）The temperature that reactor is also first adjusted before middle dropwise reaction monomer is 7 ~ 10 DEG C.
Step（2）The feed postition of middle C 5 fraction and isoamyl alkene monomer is：C 5 fraction and isoamyl alkene monomer are placed in respectively
In two dropping funels, while being added dropwise into reactor, rate of addition is controlled 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.
The modification dicyclopentadiene petroleum resin that the present embodiment is prepared is respectively according to GB 4507 ~ 1999《Pitch softens
Point determination method》、GBT22295~2008《Transparency liquid colourity is monitored》The softening point and colourity of modified petroleum resin are examined
Survey, 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
For 120 DEG C, colourity 4, melt viscosity 152cps.
The C5 Petropols that iso-amylene of the present invention is modified, by by the alkadienes copolymerization in iso-amylene and C 5 fraction
Close so that the Petropols lighter color of preparation, softening point are high, when being applied to making highway sign, graticule traffic paint, with road
Face has a higher bond strength, and with wearability is high, resistance to sunshine-duration length, the features such as antioxygenic property is good, greatly increase
The service life of traffic paint, reduces use cost, with preferable application value and prospect.
The preparation technology for the C5 Petropols that iso-amylene of the present invention is modified is simple, and reaction condition is gentle, operation side
Just, production equipment and power consumption are less, reduce production difficulty and production cost, are adapted to popularization and application.
The specific embodiment of the present 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 make various deformations or amendments within the scope of the claims, this not shadow
Ring the substance of the present invention.
Claims (9)
1. the C5 Petropols that a kind of iso-amylene is modified, it is characterised in that：Each raw material including following parts by weight：Iso-amylene 20 ~
36 parts, it is 60 ~ 85 parts of C 5 fraction, 0.1 ~ 3 part of catalyst, 80 ~ 150 parts of toluene, 0.8 ~ 1.6 part of age resistor, 0.5 ~ 2 part of alkali lye, broken
0.5 ~ 4.6 part of emulsion, also including appropriate water.
2. the C5 Petropols that iso-amylene according to claim 1 is modified, it is characterised in that：32 parts of the iso-amylene, C5
78 parts of cut, 1.2 parts of catalyst, 120 parts of toluene, 1.4 parts of age resistor, 0.9 part of alkali lye, 3.3 parts of demulsifier, also including appropriate
Water.
3. the C5 Petropols that iso-amylene according to claim 1 is modified, it is characterised in that：The C 5 fraction includes quality
Hundred contents are respectively isoprene 35% ~ 55%, pentadiene 20% ~ 40%, cyclopentadiene 5% ~ 10%, and remaining component is less than 0.1%.
4. the C5 Petropols that iso-amylene according to claim 1 is modified, it is characterised in that：The catalyst is AlCl3。
5. the C5 Petropols that iso-amylene according to claim 1 is modified, it is characterised in that：The age resistor is anti-for phenols
Old agent.
6. the method that one kind prepares the C5 Petropols that the iso-amylene as described in any one of claim 1 ~ 5 is modified, its feature exists
In：Comprise the following steps：
（1）Toluene and anhydrous Aluminum chloride are weighed respectively according to proportioning, and a small amount of toluene and anhydrous chlorination are first added into reactor
Aluminium, adds residual toluene while stirring, anhydrous Aluminum chloride is fully dissolved, and nitrogen protection is then led into reactor；
（2）C 5 fraction and isoamyl alkene monomer are weighed according to proportioning, is slowly dropped in reactor, control dropping temperature and dropwise addition speed
Degree, it is 40 ~ 60 DEG C that temperature is controlled after completion of dropwise addition, reacts 5 ~ 7.5h；
（3）Alkali lye, demulsifier and suitable quantity of water are added into reacted mixture, 30 ~ 50min is stirred in 40 ~ 60 DEG C, stands and divides
Liquid, takes supernatant liquid；
（4）Supernatant liquid is purified, unreacted monomer and other impurity is removed, that is, obtains what described iso-amylene was modified
C5 Petropols.
7. the preparation method for the C5 Petropols that iso-amylene according to claim 6 is modified, 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 for the C5 Petropols that iso-amylene according to claim 6 is modified, it is characterised in that：The step
（2）The feed postition of middle C 5 fraction and isoamyl alkene monomer is：C 5 fraction and isoamyl alkene monomer are placed in two dropping funels respectively
In, while being added dropwise into reactor, control rate of addition so that reaction monomers are in 20 ~ 30min completion of dropping.
9. the preparation method for the C5 Petropols that iso-amylene according to claim 6 is modified, it is characterised in that：The step
（4）Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710206159.2A CN106947024A (en) | 2017-03-31 | 2017-03-31 | C5 Petropols and preparation method that a kind of iso-amylene is modified |
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| CN201710206159.2A CN106947024A (en) | 2017-03-31 | 2017-03-31 | C5 Petropols and preparation method that a kind of iso-amylene is modified |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320648A (en) * | 2000-04-26 | 2001-11-07 | 上海石油化工股份有限公司 | Process for preparing C5 monoolefin modified m-pentadiene petro-resin |
| CN103382238A (en) * | 2012-05-04 | 2013-11-06 | 青岛伊科思新材料股份有限公司 | Polymerization method for m-pentadiene petroleum resin |
-
2017
- 2017-03-31 CN CN201710206159.2A patent/CN106947024A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320648A (en) * | 2000-04-26 | 2001-11-07 | 上海石油化工股份有限公司 | Process for preparing C5 monoolefin modified m-pentadiene petro-resin |
| CN103382238A (en) * | 2012-05-04 | 2013-11-06 | 青岛伊科思新材料股份有限公司 | Polymerization method for m-pentadiene petroleum resin |
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