CN110204657A - Light number a kind of, high softening-point C9 hot polymerization petroleum resin products and preparation process - Google Patents
Light number a kind of, high softening-point C9 hot polymerization petroleum resin products and preparation process Download PDFInfo
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Abstract
The invention discloses the C9 hot polymerization petroleum resin products and preparation process of a kind of light color number, high softening-point, belong to Petropols preparation technical field.Preparation method of the invention first carries out rectification process to C9 feedstock oil the following steps are included: using the byproduct C9 aromatic fraction of cracking ethylene preparation device as primary raw material, obtains de- weight C9 raw material；Treated that the substances such as C9 raw material, dicyclopentadiene, methyldicyclopentadiene, indenes and indane are dissolved in solvent naphtha for the de- weight of relationship accurate weighing according to a certain percentage again; it is then added into hot polymerization reaction kettle and reaction releaser is added; it stirs evenly; polymerization reaction is carried out under nitrogen atmosphere protection and normal pressure, the reactant after polymerization is obtained into C9 hot polymerization Petropols after stripper plant recovered solvent oil.The present invention passes through the content of certain components in allotment reaction mass, while taking and adding the C9 hot polymerization Petropols suitable for painting industry that light color number, high softening-point can be prepared in the mode for reacting releaser.
Description
Technical field
The invention belongs to Petropols preparation technical field more particularly to the C9 hot polymerization stones of a kind of light color number, high softening-point
Oleoresin product and preparation process.
Background technique
C9 hot polymerization Petropols have good adhesivity, paint and coatings industry in, Petropols can by with
Other type resins are used in mixed way, partially or completely the higher resin of alternative cost, are guaranteeing the same of quality in this way
When the physicochemical properties such as the water resistance, stability and chemical resistance that reduce cost, while improving product.Ink industry is being printed,
All multicomponents in Petropols and printing ink have good compatibility, and for the ink of different size, petroleum tree
Rouge can meet the needs of performances such as its solvent release, water resistant alkali resistance, rate of drying and wetting speed, contain petroleum simultaneously
The ink film forming of resin rapidly, can keep the dispersity of pigment stabilizer for a long time.
C9 Petropols production in the world's is substantially monopolized by the major company of the states such as West Europe, the U.S. and Japan.Wherein, the U.S. and
Japan is main C9 Petropols country of consumption, accounts for about the 2/3 of world's total sales volume.The material supplier of C9 Petropols mainly has
Lyondell company, the U.S., Exxon company, West Europe Rsm company and Dow company.External C9 petroleum resin products mainly have:
(1) routine C9 Petropols are polymerized by 140~210 DEG C of fractions in drippolene.(2) aliphatic modified aromatic resins are
Improvement and ethene-vinyl acetate copolymer it is coordinating, C9 aromatic resins C 5 fraction object is alkylated, such as styrene, second
Alkenyl toluene；The cyclopentadiene generated after dicyclopentadiene and its decomposition；Indenes and its derivative.(3) add hydrogen C9 Petropols, such as
The ArTkon resin of Japanese Arakawa company, wherein C9 aromatic resins add hydrogen partly or entirely to control its polarity.(4) pure list
Body aromatic resin is not plus the water-white resin of hydrogen, workable monomer mainly have α-methylstyrene (production of Amoco company),
Styrene (production of Hercules company), α-methylstyrene and vinyltoluene (production of Hercules company) etc..(5) it is copolymerized
Petropols are copolymerized with C9 fraction and certain C5 concentrates, have higher iodine number than coumarone indene resin or routine C9 resin, and
Dissolubility is fine, such as the Nevchem series of Neville company.(6) after polymerization resin.(7) tar resin of black, by second
Cracking aromatic tar thermal polymerization in alkene device forms.
There are three types of the synthesis mode of C9 Petropols is total, respectively thermal polymerization, catalytic polymerization, free radical polymerization.Thermal polymerization
Reaction is usually that C9 fraction is heated to 260 DEG C or so in a kettle, first by two can the molecule of polymers form Diels-
Alder addition intermediate radical, then with another can the molecule of poly group point react, generate two free radicals, then cause and polymerize.Hot polymerization
The simple process of conjunction method synthetic resin, yield are high, production gained color of resin is deep, therefore domestic is presently mainly to use the method
To produce ink industry and paint industry C9 Petropols.But the research of country's C9 hot polymerization Petropols is started late, basis
There are a certain distance for the research of property and the research of reaction mechanism are more external, while the production of country's C9 hot polymerization Petropols
Scale is more external less than normal, and the color of products obtained therefrom is relatively deep (gardner color number is mostly 11~No. 15), and lower (100 DEG C of softening point
~120 DEG C), and ink industry and paint industry are to the quality of Petropols, it is especially more stringent to softening point requirement, therefore
China is mostly external import for the Petropols of ink industry and paint industry, and this severely limits the development of domestic enterprise.
Applicant has been devoted to the research and process modification of domestic petroleum naval stores, and has applied for title in 2018
Are as follows: the patent of a kind of light color C9 hot polymerization petroleum resin products and its preparation process, this application is with cracking ethylene preparation device
Byproduct C9 aromatic fraction is primary raw material, first carries out de- weight and de- light processing to C9 feedstock oil；Then de- light processing will be taken off again
C9 raw material afterwards is mixed with dicyclopentadiene, methyldicyclopentadiene, indenes and indane, is deployed to the component of reaction mass,
So as to which the C9 hot polymerization petroleum resin products of light color number are prepared, the coloration for solving existing C9 hot polymerization Petropols is deeper
Problem.But the softening point using the technique of this application production gained C9 hot polymerization Petropols is still relatively low, it is difficult to meet oil
The use demand to the more demanding field of softening point such as ink and paint industry.
Summary of the invention
1. to solve the problems, such as
It is an object of the invention to overcome the color number using domestic prior art production gained C9 hot polymerization Petropols relatively deep,
Softening point is lower, it is difficult to which the deficiency for meeting the industries requirement such as ink and paint provides light number a kind of, high softening-point
C9 hot polymerization petroleum resin products and preparation process.The present invention is regulated and controled by the component to reaction mass, and is added centainly
It is soft to obtain light color number, height so as to effectively improve the softening point of gained C9 hot polymerization petroleum resin products for polymerization reaction releaser
Change the product of point, and then can satisfy the requirement of the industries such as ink and paint.
2. technical solution
To solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
The preparation process of the C9 hot polymerization petroleum resin products of a kind of light color number, high softening-point of the invention, to crack second processed
The byproduct C9 aromatic fraction of alkene device is primary raw material, first carries out rectification process to C9 feedstock oil, is removed in C9 feedstock oil
Heavier component；Then according to a certain percentage relationship by de- weight treated C9 raw material, dicyclopentadiene, methyl bicycle penta 2
Alkene, indenes and indenes and solvent naphtha mixing are placed in hot polymerization reaction kettle, and are added certain reaction releaser thereto and carried out hot polymerization
The C9 hot polymerization petroleum resin products of light color number, high softening-point are prepared in reaction.
Further, naphthalene when carrying out rectification process to C9 feedstock oil mainly in removing C9 raw material and other polycyclic
Aromatic hydrocarbon substance, the removing amount of heavy constituent account for about the 10%~15% of total raw material weight, preferably 12%~15%.
Further, the main component of C9 raw material is Styrene and its derivatives (5~15%), methylbenzene after de- weight
Ethylene and its derivative (10~20%), dicyclopentadiene (20~30%), indenes and indane (10~20%), methyl bicycle penta 2
Alkene (5~15%), C9 all kinds of alkane compounds (1~30%) below.
Further, the de- heavy C9 raw material, dicyclopentadiene, methyldicyclopentadiene, indenes and indane and solvent naphtha
Mixing mass ratio be (800~1200): (100~500): (50~100): (100~200): 100.
Further, the reaction releaser reacts the reactive polymeric liquid stayed in advance using last time hot polymerization, adds
Dosage accounts for the 10%~30% of reaction raw materials gross mass, preferably 15%~25%.
Further, the temperature of hot polymerization reaction is 230~260 DEG C, reaction time control 5~for 24 hours；More preferably
, the polymerization temperature is 240 DEG C~250 DEG C, and polymerization time is 10~18h.
Further, the solvent naphtha is benzene,toluene,xylene, pentane, isopentane, hexane, hexamethylene, heptan
One of alkane, octane, nonane, certain herbaceous plants with big flowers alkane, solvent D40 and solvent D60 or a variety of；The resulting polymer fluid of hot polymerization is through stripping to solvent
Oil is recycled.
The C9 hot polymerization petroleum resin products of a kind of light color number, high softening-point of the invention, the Petropols use above-mentioned side
Method is prepared.
Further, the gardner color number of the C9 hot polymerization Petropols is 9~No. 13, and softening point is 120 DEG C~140
℃。
3. beneficial effect
Compared with the prior art, the invention has the benefit that
(1) preparation process of the C9 hot polymerization petroleum resin products of a kind of light color number of the invention, high softening-point, to crack system
The byproduct C9 aromatic fraction of ethylene unit is primary raw material, is deployed by composition to C9 reaction raw materials and proportion, and
Certain reaction releaser is added, in polymerization reaction so as to which the C9 hot polymerization petroleum tree of light color number, high softening-point is prepared
Fat prod, and then can satisfy paint and graphite industry to the quality requirements of C9 Petropols.
(2) preparation process of the C9 hot polymerization petroleum resin products of a kind of light color number of the invention, high softening-point, by anti-
The additive amount for answering the group of raw material to be grouped as and react releaser is adjusted, so as to gained C9 hot polymerization petroleum resin products
Coloration and softening point regulated and controled, the gardner color number of gained naval stores can be controlled in 9~No. 13, softening point can be controlled in
120 DEG C~140 DEG C, modification scope is relatively wide.
(3) preparation process of the C9 hot polymerization petroleum resin products of a kind of light color number of the invention, high softening-point, C9 raw material warp
The heavy constituent of rectifying excision can be used for reconciling after adding hydrogen oil product, the method is easy, it is easy to operate, be suitable for it is extensive, automatically
Metaplasia produces, and contamination-free generates, and resource utilization is high.
(4) the C9 hot polymerization petroleum resin products of a kind of light color number of the invention, high softening-point, by its preparation process into
Row optimization design so as to effectively improve the softening point of the C9 hot polymerization petroleum resin products, and reduces its coloration, so as to full
Foot paint and graphite industry are to the quality requirements of C9 Petropols.
Specific embodiment
For can not produce to obtain the C9 hot polymerization stone of high-quality because of various complexity of C9 material composition in the prior art
The coloration of oleoresin, especially gained C9 hot polymerization Petropols is relatively deep, and softening point is lower, is unable to satisfy ink industry and oil
The use demand of Qi Hangye.Therefore, Petropols mostly external import of the China for ink industry and paint industry at present, this
Seriously limit the development of domestic enterprise.The present invention is optimized by the production technology to C9 hot polymerization Petropols, and one
Aspect deploys the component of C9 reaction raw materials, and certain hot polymerization C9 Petropols are on the other hand added in polymerization reaction and are made
To react releaser, so as to reduce its coloration on the basis of effectively improving gained C9 Petropols softening point.By this
The C9 hot polymerization Petropols that method is prepared, gardner color number can be controlled in 9~No. 13, softening point can be controlled in 120 DEG C~
140 DEG C, and be dissolvable in water in non-aromatic solvent naphtha, therefore the downstream client of paint and ink industry can be met to C9 hot polymerization resin
The demand of quality.
To further appreciate that the contents of the present invention, the present invention is further described below combined with specific embodiments below, but
Because length is limited, case study on implementation is only enumerated below, and range is not limited to the design parameter in following embodiment.
Embodiment 1
C9 raw material is subjected to distillation processing first, removes heavier component 15% (accounting for C9 total mass of raw material) in C9 raw material.So
Weigh de- weight respectively afterwards treated C9 raw material 1000g, dicyclopentadiene 250g, methyldicyclopentadiene 50g, indenes and indane
100g is simultaneously dissolved in 100g solvent naphtha；20% reaction releaser is added to reaction kettle, then reaction mass is added
It in hot polymerization reaction kettle and stirs evenly, under nitrogen atmosphere protection and normal pressure, the reaction temperature for controlling polymerization is 240 DEG C, when reaction
Between control in 16h, after which the reaction product of polymerization to be obtained to C9 hot polymerization Petropols after strip recovered solvent oil after reaction.It surveys
The gardner color number for obtaining resin is 10#, and softening point is 135.2 DEG C.
Embodiment 2
C9 raw material is subjected to distillation processing first, removes heavier component 12% (accounting for C9 total mass of raw material) in C9 raw material.So
Weigh de- weight respectively afterwards treated C9 raw material 800g, dicyclopentadiene 400g, methyldicyclopentadiene 70g, indenes and indane
130g is simultaneously dissolved in 100g solvent naphtha；26% reaction releaser is added to reaction kettle, then reaction mass is added
It in hot polymerization reaction kettle and stirs evenly, under nitrogen atmosphere protection and normal pressure, the reaction temperature for controlling polymerization is 245 DEG C, when reaction
Between control in 18h, after which the reaction product of polymerization to be obtained to C9 hot polymerization Petropols after strip recovered solvent oil after reaction.It surveys
The gardner color number for obtaining resin is 12#, and softening point is 140.3 DEG C.
Embodiment 3
C9 raw material is subjected to distillation processing first, removes heavier component 15% (accounting for C9 total mass of raw material) in C9 raw material.So
Weigh de- weight respectively afterwards treated C9 raw material 1100g, dicyclopentadiene 100g, methyldicyclopentadiene 100g, indenes and indane
100g is simultaneously dissolved in 100g solvent naphtha；25% reaction releaser is added to reaction kettle, then reaction mass is added
It in hot polymerization reaction kettle and stirs evenly, under nitrogen atmosphere protection and normal pressure, the reaction temperature for controlling polymerization is 240 DEG C, when reaction
Between control in 12h, after which the reaction product of polymerization to be obtained to C9 hot polymerization Petropols after strip recovered solvent oil after reaction.It surveys
The gardner color number for obtaining resin is 9#, and softening point is 128.2 DEG C.
Embodiment 4
C9 raw material is subjected to distillation processing first, removes heavier component 13% (accounting for C9 total mass of raw material) in C9 raw material.So
Weigh de- weight respectively afterwards treated C9 raw material 900g, dicyclopentadiene 300g, methyldicyclopentadiene 50g, indenes and indane
150g is simultaneously dissolved in 100g solvent naphtha；30% reaction releaser is added to reaction kettle, then reaction mass is added
It in hot polymerization reaction kettle and stirs evenly, under nitrogen atmosphere protection and normal pressure, the reaction temperature for controlling polymerization is 250 DEG C, when reaction
Between control in 10h, after which the reaction product of polymerization to be obtained to C9 hot polymerization Petropols after strip recovered solvent oil after reaction.It surveys
The gardner color number for obtaining resin is 13#, and softening point is 138.1 DEG C.
Embodiment 5
C9 raw material is subjected to distillation processing first, removes heavier component 10% (accounting for C9 total mass of raw material) in C9 raw material.So
Weigh de- weight respectively afterwards treated C9 raw material 1200g, dicyclopentadiene 500g, methyldicyclopentadiene 80g, indenes and indane
200g is simultaneously dissolved in 100g solvent naphtha；15% reaction releaser is added to reaction kettle, then reaction mass is added
It in hot polymerization reaction kettle and stirs evenly, under nitrogen atmosphere protection and normal pressure, the reaction temperature for controlling polymerization is 247 DEG C, when reaction
Between control in 14h, after which the reaction product of polymerization to be obtained to C9 hot polymerization Petropols after strip recovered solvent oil after reaction.It surveys
The gardner color number for obtaining resin is 12#, and softening point is 135 DEG C.
Claims (9)
1. a kind of preparation process of the C9 hot polymerization petroleum resin products of light color number, high softening-point, it is characterised in that: to crack second processed
The byproduct C9 aromatic fraction of alkene device is primary raw material, first carries out rectification process to C9 feedstock oil, is removed in C9 feedstock oil
Heavier component；Then according to a certain percentage relationship by de- weight treated C9 raw material, dicyclopentadiene, methyl bicycle penta 2
Alkene, indenes and indenes and solvent naphtha mixing are placed in hot polymerization reaction kettle, and are added certain reaction releaser thereto and carried out hot polymerization
The C9 hot polymerization petroleum resin products of light color number, high softening-point are prepared in reaction.
2. the preparation process of the C9 hot polymerization petroleum resin products of a kind of light color number according to claim 1, high softening-point,
It is characterized in that: mainly removing the naphthalene and other multiring aromatic hydrocarbon objects in C9 raw material when carrying out rectification process to C9 feedstock oil
Matter, the removing amount of heavy constituent account for about the 10%~15% of total raw material weight, preferably 12%~15%.
3. the preparation process of the C9 hot polymerization petroleum resin products of a kind of light color number according to claim 1, high softening-point,
Be characterized in that: the main component of C9 raw material is Styrene and its derivatives (5~15%), methyl styrene and its spreads out after de- weight
Biological (10~20%), dicyclopentadiene (20~30%), indenes and indane (10~20%), methyldicyclopentadiene (5~
15%), C9 all kinds of alkane compounds (1~30%) below.
4. the C9 hot polymerization petroleum resin products of a kind of light color number according to any one of claim 1-3, high softening-point
Preparation process, it is characterised in that: the de- heavy C9 raw material, dicyclopentadiene, methyldicyclopentadiene, indenes and indane and solvent naphtha
Mixing mass ratio be (800~1200): (100~500): (50~100): (100~200): 100.
5. the C9 hot polymerization petroleum resin products of a kind of light color number according to any one of claim 1-3, high softening-point
Preparation process, it is characterised in that: the reaction releaser reacts the reactive polymeric liquid stayed in advance using last time hot polymerization, adds
Dosage accounts for the 10%~30% of reaction raw materials gross mass, preferably 15%~25%.
6. the C9 hot polymerization petroleum resin products of a kind of light color number according to any one of claim 1-3, high softening-point
Preparation process, it is characterised in that: the temperature of hot polymerization reaction is 230~260 DEG C, reaction time control 5~for 24 hours；It is more excellent
Choosing, the polymerization temperature is 240 DEG C~250 DEG C, and polymerization time is 10~18h.
7. the C9 hot polymerization petroleum resin products of a kind of light color number according to any one of claim 1-3, high softening-point
Preparation process, it is characterised in that: the solvent naphtha is benzene,toluene,xylene, pentane, isopentane, hexane, hexamethylene, heptan
One of alkane, octane, nonane, certain herbaceous plants with big flowers alkane, solvent D40 and solvent D60 or a variety of；The resulting polymer fluid of hot polymerization is through stripping to solvent
Oil is recycled.
8. the C9 hot polymerization petroleum resin products of a kind of light color number, high softening-point, it is characterised in that: the Petropols are wanted using right
Method described in any one of 1-7 is asked to be prepared.
9. the C9 hot polymerization petroleum resin products of a kind of light color number according to claim 8, high softening-point, it is characterised in that:
The gardner color number of the C9 hot polymerization Petropols is 9~No. 13, and softening point is 120 DEG C~140 DEG C.
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| CN114539475A (en) * | 2022-03-30 | 2022-05-27 | 抚顺市裕龙化工有限公司 | Thermal polymerization process of carbon-nine petroleum resin |
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