CN110183577A - A kind of cold poly- petroleum resin products of light color C9 and its preparation process - Google Patents
A kind of cold poly- petroleum resin products of light color C9 and its preparation process Download PDFInfo
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Abstract
The invention discloses a kind of cold poly- petroleum resin products of light color C9 and preparation processes, belong to Petropols preparation technical field.Preparation method of the invention is the following steps are included: with the byproduct C9 aromatic fraction of cracking ethylene preparation device or resinon or combinations thereof for primary raw material, rectification process first is carried out to feedstock oil, remove the heavier component and lighter component in C9 feedstock oil, then feedstock oil is subjected to prepolymerization, removes the higher component of reactivity in reaction raw materials；Treated that the substances such as raw material, indenes and indane, styrene, methyl styrene are dissolved in solvent naphtha for relationship accurate weighing according to a certain percentage again, catalytic polymerization is carried out, the reactant after polymerization is obtained into the cold poly- Petropols of chrominance C 9 after the techniques such as alkali cleaning, washing, stripping.The present invention is by the component of the cold poly- Petropols color of certain influence C9 in excision C9 raw material, then deploys the content of key component in reaction mass the cold poly- Petropols of light color C9 can be prepared.
Description
Technical field
The invention belongs to Petropols preparation technical field more particularly to a kind of cold poly- petroleum resin products of light color C9 and
Its preparation process.
Background technique
The raw material pyrolysis c9 fraction of Petropols is that boiling point more than 150 kinds of aromatic components of range within 240 DEG C are answered
Miscellaneous mixture disperses without fixed composition, and very, is not readily separated.From the angle of synthesis, two classes can be divided into,
A kind of is the active component that can carry out polymerization reaction, such as: styrene and vinyltoluene class, dicyclopentadiene；It is another kind of
For inactive ingredients, such as alkylbenzene and condensed-nuclei aromatics, solvent can be played the role of in polymerization, be distilled out again after reaction
Come.About 50% polymer monomer is typically contained in C9 raw material, unsaturated olefin is rich in, so that C9 fraction be made to be suitble to produce
The raw material of Petropols.
There are three types of the synthesis mode of C9 Petropols is total, respectively thermal polymerization, catalytic polymerization and free radical polymerization.Wherein,
The polymerization processes therewith of C9 Petropols is otherwise known as cationic polymerization technique, the cationic initiated polymerization mistake of Petropols
Journey, mainly C9 monomer generate carbocation active group under the action of acid cation initiator, then cause chain type rapidly
Increase sudden reaction, it is final to obtain the cold poly- Petropols of C9.Currently, cationic polymerization mostly uses concentrated acid (sulfuric acid, phosphoric acid or mixed
Acid etc.), the metal halides such as Lewis acid boron trifluoride or alchlor be initiator, polymerization temperature section is generally 0~100
℃.The reaction rate of this synthetic method is high, reaction temperature is low, energy consumption cost is low and operating procedure is simple, at the same time institute
Resin high income, form and aspect are relatively shallower, product quality is high.
Corresponding to different polymerizing conditions, the Petropols of synthesis also have a different physicochemical properties, and Petropols
Application field depends primarily on the multinomial performance index that resin itself has, and generally comprises following Index Content: softening point, color
Phase, bromine number, acid value, specific gravity, melt viscosity, ash content, normal heptane value and pH value etc..Wherein, the cold poly- Petropols of C9 are mainly answered
For painting, the industries such as ink, adhesive.Currently, there are the enterprise of more than 50 production Petropols, production gained stone in the country, China
C9 Aromatic Petroleum Resins account for 70% production capacity share in oleoresin, but compared with the enterprise of external production Petropols, state
Interior kind model is more single, and product quality level is lower, and the especially main performances such as the coloration of product, softening point not can be carried out
Effectively control.In recent years, domestic Petropols market demand is increasing sharply, be especially largely used to rubber processing,
The annual demand growth rate of the multi-field Petropols such as paint, ink, adhesive is surprising, but due to C9 fraction at
Divide complexity, and boiling point is higher, it is difficult to it is precisely separated, the domestic market production gained cold poly- petroleum resin products of C9
Coloration is mostly 6~No. 8 colors, it is difficult to which production obtains the lighter number cold poly- Petropols of C9, to be difficult to meet certain lower tourists
Family, such as the demand of amenities, environmental supplies field to the cold poly resin of light color C9.
Through retrieving, the application case that Chinese Patent Application No. is 201110240527.8 discloses a kind of light color degree aromatic series stone
The preparation method of oleoresin, this application crack heavy distillat (cracking of ethylene by-product C9 double distilled with the 2# of cracking of ethylene by-product
Point) be raw material, isolate resin liquid fraction through rectifying, then resin liquid fraction is decolourized, is polymerize, Removal of catalyst and point
Separating process processing, so as to which the light aromatic petroleum resin of coloration < 1# is prepared.But mainly pass through in this application
It adds certain decolorising agent and decolorization is carried out to resin liquid fraction to reduce the coloration of gained petroleum resin products, but gained tree
The Colour range of fat prod is relatively narrow, and is not easy to carry out accuracy controlling to the coloration of naval stores.
Summary of the invention
1. to solve the problems, such as
It is an object of the invention to overcome the coloration for using prior art to produce the gained cold poly- petroleum resin products of C9 opposite
It is relatively deep, it is difficult to which that the deficiency for meeting the use demand of the fields such as amenities, environmental supplies poly- Petropols cold to light color C9 mentions
A kind of cold poly- petroleum resin products of light color C9 and its preparation process are supplied.It is final obtained using technical solution of the present invention
The gardner color number of the cold poly- Petropols of C9 can be controlled in 2~No. 5, to meet downstream client to the cold poly resin of light color C9
Demand.2. technical solution
To solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
A kind of preparation process of the cold poly- petroleum resin products of light color C9 of the invention, comprising the following steps:
Step 1: rectification process
Rectification process is carried out to C9 raw material, to remove the heavy constituent and part light component in C9 feedstock oil；
Step 2: prepolymerization
Feedstock oil after rectification process is subjected to prepolymerization, to remove the higher component of reactivity in reaction raw materials；
Step 3: catalytic polymerization
By prepolymerization treated raw material and Styrene and its derivatives, methyl styrene and its derivative, indenes and its spread out
Biology and methyl indenes carry out catalytic polymerization together, so that the cold poly- petroleum resin products of light color C9 be prepared.
Further, the temperature of the prepolymerization is -10~30 DEG C, and the reaction time is 1~5h, the use of catalyst
Amount is 0~1%；It is furthermore preferred that the temperature of the prepolymerization is 0~20 DEG C, the reaction time is 1~2h, the use of catalyst
Amount is 0.1%~0.5%.
Further, in the catalytic polymerization, Styrene and its derivatives, methylbenzene in final gained reaction solution
The quality of ethylene and its derivative, indenes and its derivative, methyl indenes account for respectively polymerization liquid total amount percentage be 15~
35%, 5~20%, 5~20%, 5~10%.
Further, the reaction temperature of the catalytic polymerization is 0~50 DEG C, and the reaction time is 1~5h, catalyst
Dosage be 0.1~1%；It is furthermore preferred that the reaction temperature of catalytic polymerization is 10 DEG C~30 DEG C, the reaction time is 2~3h,
The dosage of catalyst is 0.4%~0.8%.
Further, the heavy constituent that rectification process removes in step 1 mainly includes naphthalene and other polycyclic aromatic hydrocarbons, removing
Light component mainly include dicyclopentadiene, methyldicyclopentadiene, cyclopentadiene and methyl cyclopentadiene, and above-mentioned heavy constituent
Account for 10%~15%, the 5%~15% of C9 raw material gross weight respectively with the removing amount of light component, removing amount difference is further preferred
It is 12%~15%, 7%~12%.
Further, the component of prepolymerization processing removing is mainly remaining bicyclic penta 2 after rectifying in step 2
Alkene, methyldicyclopentadiene and its derivative, the removing amount of above-mentioned active component account for the 5%~15% of C9 raw material gross weight, preferably
It is 7%~12%.
Further, the C9 raw material is using in the byproduct C9 aromatic fraction of cracking ethylene preparation device, resinon
It is one or more.
Further, all reaction raw materials are dissolved in solvent naphtha in step 3, it then will by the way of being added dropwise
It is added in reaction kettle and carries out catalytic polymerization, and by obtained reactant through urging in alkali cleaning, washing process elimination reaction stoste
Agent component, soda-wash solution used are sodium hydroxide solution, in potassium hydroxide solution, calcium hydroxide solution, ammonia spirit
It is one or more.
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 cold poly- petroleum resin products of a kind of light color C9 of the invention, the petroleum resin products use method system of the invention
Standby to obtain, gardner color number is 2~No. 5.
3. beneficial effect
Compared with the prior art, the invention has the benefit that
(1) preparation process of the cold poly- petroleum resin products of a kind of light color C9 of the invention, at rectifying and prepolymerization
Reason to cut off certain components in C9 raw material, and be added Styrene and its derivatives, methyl styrene and its derivative, indenes and its
Derivative and methyl indenes deploy raw material components, produce so as to produce to obtain the cold poly- Petropols of C9 of lower coloration
The gardner color number of product, gained C9 petroleum resin products can be controlled in 2~No. 5, to meet the spies such as health product, environment-friendly products
Demand of the different field to light degree petroleum resin products.
(2) preparation process of the cold poly- petroleum resin products of a kind of light color C9 of the invention, removes C9 by rectification process
Naphthalene and other polycyclic aromatic hydrocarbon heavy constituents and dicyclopentadiene, methyldicyclopentadiene, cyclopentadiene and methyl in feedstock oil
The high activities light component such as cyclopentadiene, and by carrying out pre-polymerization processing to feedstock oil after rectification process, so as to effectively de-
Except a small amount of dicyclopentadiene remaining after rectifying, methyldicyclopentadiene and its derivative isoreactivity higher composition, so it is advantageous
In the coloration for reducing the final gained cold poly- petroleum resin products of C9.
(3) preparation process of the cold poly- petroleum resin products of a kind of light color C9 of the invention, by prepolymerization and finally
The proportion of the polymerization temperature of polymerization processes therewith, time and each ingredient carries out strict control, to advantageously ensure that final institute
The coloration for obtaining product can satisfy demand of the fields such as health product, environment-friendly products to light degree petroleum resin products；Meanwhile it is logical
It crosses and the proportion of each component is adjusted, additionally it is possible to the coloration of gained petroleum resin products is adjusted, adjustable range is opposite
It is wider, so as to meet the use demand of different field.
(4) preparation process of the cold poly- petroleum resin products of a kind of light color C9 of the invention, the heavy constituent that raw material is cut off
It can be used for reconciling oil product after adding hydrogen, and light component can also be sold outside after processing；This method is easy, it is easy to operate, be suitable for it is big
Scale, automated production, and contamination-free generates, and resource utilization is high.
(5) the cold poly- petroleum resin products of a kind of light color C9 of the invention, by being optimized to its preparation process, thus
It can effectively reduce its coloration, the coloration of the cold poly- petroleum resin products of the C9 can be controlled in 2~No. 5, to meet certain special necks
The demand of domain poly- Petropols cold to light color C9.
Specific embodiment
It is relatively deep for the coloration of the cold poly- petroleum resin products of existing C9, it is difficult to meet amenities, environmental supplies etc.
The problem of use demand of field poly- Petropols cold to light color C9, the present invention cut off C9 by rectifying and prepolymerization processing
Certain components in raw material, and Styrene and its derivatives, methyl styrene and its derivative, indenes and its derivative and first is added
Base indenes deploys raw material components, controls final gained reactant material, i.e., Styrene and its derivatives, first in polymerization liquid
Base Styrene and its derivatives, indenes and its derivative, methyl indenes and other alkanes components are (including other in pre-polymerization C9 raw material
Alkane component in alkane component and solvent naphtha) quality account for respectively polymerization liquid total amount percentage be 15~35%, 5~
20%, 5~20%, 5~10% and 30~45%, so as to which the coloration of gained petroleum resin products is effectively reduced, produce institute
The gardner color number for obtaining C9 petroleum resin products can be controlled in 2~No. 5, and then can satisfy the spies such as health product, environment-friendly products
Demand of the different field to light degree petroleum resin products.
The present invention is further described below combined with specific embodiments below.
Embodiment 1
It uses the byproduct C9 aromatic fraction of ethylene unit for primary raw material first, first carries out the C9 raw material of 1000.00g
Rectification process, remove C9 raw material in lighter component (mainly include dicyclopentadiene, methyldicyclopentadiene, cyclopentadiene and
Methyl cyclopentadiene) about 100g, remove heavier component (mainly including naphthalene and other polycyclic aromatic hydrocarbons) about 140g in C9 raw material.So
By treated, raw material is added in reaction kettle afterwards, and the temperature of reaction kettle is set as 15 DEG C, and catalyst BF is added into reaction kettle3About
2.28g takes out after reacting 1.5h, oil product part in prepolymerization liquid is steamed, raw material (the part oil steamed after obtaining pre-polymerization
Product) about 680g.
Then weigh respectively through rectifying, pre-polymerization treated C9 raw material and pure styrene, methyl styrene and its derivative,
Indenes and indane, methyl indeno are dissolved in solvent naphtha (benzene), guarantee that styrene-content is 30% in final ingredient, methylbenzene
The content of ethylene and its derivative is 12%, and the content of indenes and indane is 12%, and the content of methyl indenes is 8%, other alkanes
Constituent content is 38%；Reaction raw materials are added in reaction kettle in a manner of being added dropwise and are stirred evenly, the dosage of catalyst is
0.6% (accounting for reaction raw materials gross mass), the reaction temperature for controlling polymerization is 20 DEG C, and reaction time control is in 2.5h, wait react knot
Polymer fluid is obtained to the cold poly- Petropols of C9 after beam after alkali cleaning, washing, stripping.Measure the gardner color of resin obtained by the present embodiment
Number be 3, softening point be 125.2 DEG C.
Embodiment 2
The byproduct C9 aromatic fraction and 500g resinon for weighing 500g ethylene unit first are primary raw material, first by raw material
Rectification process is carried out, the lighter component about 80g in raw material is removed, removes the heavier component about 130g in C9 raw material.It then will place
Raw material after reason is added in reaction kettle, and the temperature of reaction kettle is set as 20 DEG C, and it is poly- that catalyst boron trifluoride is added into reaction kettle
Ether about 2.37g takes out after reacting 2.0h, oil product part in prepolymerization liquid is steamed, the about 750g of the raw material after pre-polymerization.
Then weigh respectively through rectifying, pre-polymerization treated C9 raw material and pure styrene, methyl styrene and its derivative,
Indenes and indane, methyl indeno are dissolved in solvent naphtha (toluene), guarantee that styrene-content is 30% in final ingredient, methyl
The content of Styrene and its derivatives is 10%, and the content of indenes and indane is 10%, and the content of methyl indenes is 9%, other alkane
Class constituent content is 41%；Reaction raw materials are added in reaction kettle in a manner of being added dropwise and are stirred evenly, the dosage of catalyst is
0.8% (accounting for reaction raw materials gross mass), the reaction temperature for controlling polymerization is 25 DEG C, and reaction time control is in 2.0h, wait react knot
Polymer fluid is obtained to the cold poly- Petropols of C9 after beam after alkali cleaning, washing, stripping.Measure the gardner color of resin obtained by the present embodiment
Number be 2, softening point be 118.7 DEG C.
Embodiment 3
It uses the byproduct C9 aromatic fraction of ethylene unit for primary raw material first, first carries out the C9 raw material of 1000.00g
Rectification process removes the lighter component about 75g in C9 raw material, removes the heavier component about 125g in C9 raw material.It then will processing
Raw material afterwards is added in reaction kettle, and the temperature of reaction kettle is set as 10 DEG C, and catalyst BF is added into reaction kettle3About 1.6g, instead
It is taken out after answering 1.0h, oil product part in prepolymerization liquid is steamed, the about 740g of the raw material after pre-polymerization.
Then weigh respectively through rectifying, pre-polymerization treated C9 raw material and pure styrene, methyl styrene and its derivative,
Indenes and indane, methyl indeno are dissolved in solvent naphtha (pentane), guarantee that styrene-content is 25% in final ingredient, first
The content of base Styrene and its derivatives is 13%, and the content of indenes and indane is 13%, and the content of methyl indenes is 10%, other alkane
Hydrocarbon component content is 39%；Reaction raw materials are added in reaction kettle in a manner of being added dropwise and are stirred evenly, the dosage of catalyst
For 0.5% (accounting for reaction raw materials gross mass), the reaction temperature for controlling polymerization is 15 DEG C, and the reaction time controls in 3.0h, wait react
After by polymer fluid after alkali cleaning, washing, stripping the cold poly- Petropols of C9.Measure the Gardner of resin obtained by the present embodiment
Color number is 4, and soft bad point is 128.6 DEG C.
Embodiment 4
It uses the byproduct C9 aromatic fraction of ethylene unit for primary raw material first, first carries out the C9 raw material of 1000.00g
Rectification process removes the lighter component about 70g in C9 raw material, removes the heavier component about 125g in C9 raw material.It then will processing
Raw material afterwards is added in reaction kettle, and the temperature of reaction kettle is set as 15 DEG C, and catalyst BF is added into reaction kettle3About 2.28g, instead
It is taken out after answering 1.5h, oil product part in prepolymerization liquid is steamed, the about 750g of the raw material after pre-polymerization.
Then weigh respectively through rectifying, pre-polymerization treated C9 raw material and pure styrene, methyl styrene and its derivative,
Indenes and indane, methyl indeno are dissolved in solvent naphtha (hexane), guarantee that styrene-content is 24% in final ingredient, methyl
The content of Styrene and its derivatives is 15%, and the content of indenes and indane is 15%, and the content of methyl indenes is 9%, other alkane
Class constituent content is 37%；Reaction raw materials are added in reaction kettle in a manner of being added dropwise and are stirred evenly, the dosage of catalyst is
0.8% (accounting for reaction raw materials gross mass), the reaction temperature for controlling polymerization is 27 DEG C, and reaction time control is in 2.5h, wait react knot
Polymer fluid is obtained to the cold poly- Petropols of C9 after beam after alkali cleaning, washing, stripping.Measure the gardner color of resin obtained by the present embodiment
Number be 5, softening point be 132.6 DEG C.
Embodiment 5
It uses the byproduct C9 aromatic fraction of ethylene unit for primary raw material first, first carries out the C9 raw material of 1000.00g
Rectification process removes the lighter component about 50g in C9 raw material, removes the heavier component about 100g in C9 raw material.It then will processing
Raw material afterwards is added in reaction kettle, and the temperature of reaction kettle is set as 25 DEG C, and catalyst BF is added into reaction kettle3About 9.5g, instead
It is taken out after answering 1h, oil product part in prepolymerization liquid is steamed, the about 710g of the raw material after pre-polymerization.
Then weigh respectively through rectifying, pre-polymerization treated C9 raw material and pure styrene, methyl styrene and its derivative,
Indenes and indane, methyl indeno are dissolved in solvent naphtha (octane), guarantee that styrene-content is 15% in final ingredient, methyl
The content of Styrene and its derivatives is 20%, and the content of indenes and indane is 20%, and the content of methyl indenes is 5%, other alkane
Class constituent content is 40%；Reaction raw materials are added in reaction kettle in a manner of being added dropwise and are stirred evenly, the dosage of catalyst is
1.0% (accounting for reaction raw materials gross mass), the reaction temperature for controlling polymerization is 45 DEG C, and the reaction time controls in 1h, to the end of reacting
Polymer fluid is obtained to the cold poly- Petropols of C9 after alkali cleaning, washing, stripping afterwards.Measure the gardner color number of resin obtained by the present embodiment
It is 4, softening point is 125.3 DEG C.
Embodiment 6
It uses the byproduct C9 aromatic fraction of ethylene unit for primary raw material first, first carries out the C9 raw material of 1000.00g
Rectification process removes the lighter component about 120g in C9 raw material, removes the heavier component about 150g in C9 raw material.It then will processing
Raw material afterwards is added in reaction kettle, and the temperature of reaction kettle is set as 18 DEG C, and catalyst BF is added into reaction kettle3About 3.25g, instead
It is taken out after answering 1.5h, oil product part in prepolymerization liquid is steamed, the about 708g of the raw material after pre-polymerization.
Then weigh respectively through rectifying, pre-polymerization treated C9 raw material and pure styrene, methyl styrene and its derivative,
Indenes and indane, methyl indeno are dissolved in solvent naphtha (dimethylbenzene), guarantee that styrene-content is 35% in final ingredient, first
The content of base Styrene and its derivatives is 20%, and the content of indenes and indane is 5%, and the content of methyl indenes is 10%, other alkane
Hydrocarbon component content is 30%；Reaction raw materials are added in reaction kettle in a manner of being added dropwise and are stirred evenly, the dosage of catalyst
For 0.4% (accounting for reaction raw materials gross mass), the reaction temperature for controlling polymerization is 10 DEG C, and the reaction time controls in 2.5h, wait react
After by polymer fluid after alkali cleaning, washing, stripping the cold poly- Petropols of C9.Measure the Gardner of resin obtained by the present embodiment
Color number is 2, and softening point is 121.6 DEG C.
Embodiment 7
It uses the byproduct C9 aromatic fraction of ethylene unit for primary raw material first, first carries out the C9 raw material of 1000.00g
Rectification process removes the lighter component about 150g in C9 raw material, removes the heavier component about 120g in C9 raw material.It then will processing
Raw material afterwards is added in reaction kettle, and the temperature of reaction kettle is set as 30 DEG C, and catalyst BF is added into reaction kettle3About 4.95g, instead
It is taken out after answering 1h, oil product part in prepolymerization liquid is steamed, the about 725g of the raw material after pre-polymerization.
Then weigh respectively through rectifying, pre-polymerization treated C9 raw material and pure styrene, methyl styrene and its derivative,
Indenes and indane, methyl indeno are dissolved in solvent naphtha (hexamethylene), guarantee that styrene-content is 25% in final ingredient, first
The content of base Styrene and its derivatives is 5%, and the content of indenes and indane is 17%, and the content of methyl indenes is 8%, other alkane
Class constituent content is 45%；Reaction raw materials are added in reaction kettle in a manner of being added dropwise and are stirred evenly, the dosage of catalyst is
0.3% (accounting for reaction raw materials gross mass), the reaction temperature for controlling polymerization is 35 DEG C, and the reaction time controls in 4h, to the end of reacting
Polymer fluid is obtained to the cold poly- Petropols of C9 after alkali cleaning, washing, stripping afterwards.Measure the gardner color number of resin obtained by the present embodiment
It is 3, softening point is 119.5 DEG C.
Claims (10)
1. a kind of preparation process of the cold poly- petroleum resin products of light color C9, which comprises the following steps:
Step 1: rectification process
Rectification process is carried out to C9 raw material, to remove the heavy constituent and part light component in C9 feedstock oil；
Step 2: prepolymerization
Feedstock oil after rectification process is subjected to prepolymerization, to remove the higher component of reactivity in reaction raw materials；
Step 3: catalytic polymerization
By prepolymerization treated raw material and Styrene and its derivatives, methyl styrene and its derivative, indenes and its derivative
Catalytic polymerization is carried out together with after the mixing of methyl indenes, so that the cold poly- petroleum resin products of light color C9 be prepared.
2. a kind of preparation process of the cold poly- petroleum resin products of light color C9 according to claim 1, it is characterised in that: institute
The temperature for stating prepolymerization is -10~30 DEG C, and the reaction time is 1~5h, and the dosage of catalyst is 0~1%；It is furthermore preferred that
The temperature of the prepolymerization is 0~20 DEG C, and the reaction time is 1~2h, and the dosage of catalyst is 0.1%~0.5%.
3. a kind of preparation process of the cold poly- petroleum resin products of light color C9 according to claim 1, it is characterised in that: institute
State in catalytic polymerization, Styrene and its derivatives, methyl styrene and its derivative in final gained reaction solution, indenes and its
Derivative, methyl indenes quality account for respectively polymerization liquid total amount percentage be 15~35%, 5~20%, 5~20%, 5~
10%.
4. a kind of preparation process of the cold poly- petroleum resin products of light color C9 according to claim 1, it is characterised in that: institute
The reaction temperature for stating catalytic polymerization is 0~50 DEG C, and the reaction time is 1~5h, and the dosage of catalyst is 0.1~1%；It is more excellent
Choosing, the reaction temperature of catalytic polymerization is 10 DEG C~30 DEG C, and the reaction time is 2~3h, the dosage of catalyst is 0.4%~
0.8%.
5. a kind of preparation process of the cold poly- petroleum resin products of light color C9 described in any one of -4 according to claim 1,
Be characterized in that: the heavy constituent that rectification process removes in step 1 mainly includes naphthalene and other polycyclic aromatic hydrocarbons, the light component master of removing
It to include dicyclopentadiene, methyldicyclopentadiene, cyclopentadiene and methyl cyclopentadiene, and above-mentioned heavy constituent and light component
Removing amount accounts for 10%~15%, the 5%~15% of C9 raw material gross weight respectively, the removing amount respectively be more preferably 12%~
15%, 7%~12%.
6. a kind of preparation process of the cold poly- petroleum resin products of light color C9 described in any one of -4 according to claim 1,
It is characterized in that: the component predominantly remaining dicyclopentadiene, methyl bicycle after rectifying of prepolymerization processing removing in step 2
Pentadiene and its derivative, the removing amount of above-mentioned active component account for the 5%~15% of C9 raw material gross weight, and preferably 7%~12%.
7. a kind of preparation process of the cold poly- petroleum resin products of light color C9 described in any one of -4 according to claim 1,
Be characterized in that: the C9 raw material is using one of the byproduct C9 aromatic fraction of cracking ethylene preparation device, resinon or it is mixed
Close object.
8. a kind of preparation process of the cold poly- petroleum resin products of light color C9 described in any one of -4 according to claim 1,
It is characterized in that: all reaction raw materials being dissolved in solvent naphtha in step 3, be then added into reaction by the way of being added dropwise
Catalytic polymerization is carried out in kettle, and by obtained reactant through the catalytic component in alkali cleaning, washing process elimination reaction stoste, institute
Soda-wash solution is one of sodium hydroxide solution, potassium hydroxide solution, calcium hydroxide solution, ammonia spirit or a variety of.
9. a kind of preparation process of the cold poly- petroleum resin products of light color C9 described in any one of -4 according to claim 1,
Be characterized in that: the solvent naphtha is benzene,toluene,xylene, pentane, isopentane, hexane, hexamethylene, heptane, octane, nonyl
One of alkane, certain herbaceous plants with big flowers alkane, solvent D40 and solvent D60 or a variety of.
10. a kind of cold poly- petroleum resin products of light color C9, it is characterised in that: the petroleum resin products use claim 1-9
Any one of described in method be prepared, gardner color number be 2~No. 5.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112063102A (en) * | 2020-10-27 | 2020-12-11 | 安徽同心新材料科技有限公司 | Petroleum resin with excellent ageing resistance and preparation method thereof |
| CN113336891A (en) * | 2021-06-22 | 2021-09-03 | 大庆华科股份有限公司 | Methyl styrene and indene modified dicyclopentadiene petroleum resin and preparation method thereof |
| CN113461859A (en) * | 2021-07-02 | 2021-10-01 | 青岛海伊诺新材料科技有限公司 | Preparation method of light-colored cold-polymerized C5/C9 copolymerized petroleum resin |
| CN114395077A (en) * | 2021-12-28 | 2022-04-26 | 恒河材料科技股份有限公司 | Preparation method of naphthenic filling oil |
| CN114573752A (en) * | 2022-03-11 | 2022-06-03 | 广东新华粤石化集团股份公司 | Modified petroleum resin with narrow molecular weight distribution, preparation method and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382261A (en) * | 2011-08-22 | 2012-03-21 | 天津市兴源化工有限公司 | Preparation method for light-chroma aromatic petroleum resin |
| CN102746460A (en) * | 2012-06-27 | 2012-10-24 | 宁波职业技术学院 | Method for preparing cold-polymerized indene resin with high softening point and light color |
| CN102746459A (en) * | 2012-06-27 | 2012-10-24 | 宁波职业技术学院 | Preparation method of cold polymerized styrene-indene resin |
| CN102757530A (en) * | 2012-06-27 | 2012-10-31 | 宁波职业技术学院 | Preparation method of light-color cold polymerized C9 petroleum resin |
| CN109400806A (en) * | 2018-09-21 | 2019-03-01 | 安徽同心化工有限公司 | A kind of light color C9 hot polymerization petroleum resin products and its preparation process |
-
2019
- 2019-06-18 CN CN201910524465.XA patent/CN110183577A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382261A (en) * | 2011-08-22 | 2012-03-21 | 天津市兴源化工有限公司 | Preparation method for light-chroma aromatic petroleum resin |
| CN102746460A (en) * | 2012-06-27 | 2012-10-24 | 宁波职业技术学院 | Method for preparing cold-polymerized indene resin with high softening point and light color |
| CN102746459A (en) * | 2012-06-27 | 2012-10-24 | 宁波职业技术学院 | Preparation method of cold polymerized styrene-indene resin |
| CN102757530A (en) * | 2012-06-27 | 2012-10-31 | 宁波职业技术学院 | Preparation method of light-color cold polymerized C9 petroleum resin |
| CN109400806A (en) * | 2018-09-21 | 2019-03-01 | 安徽同心化工有限公司 | A kind of light color C9 hot polymerization petroleum resin products and its preparation process |
Non-Patent Citations (3)
| Title |
|---|
| 《化工百科全书》编辑委员会: "《化工百科全书 第16卷 天然药物-无机过氧化物和过氧化和物》", 31 December 1997, 第269页 * |
| 吴利红，等: "活性组分含量对阳离子聚合C9石油树脂的影响", 《化学工业与工程》 * |
| 梁受天: "C9馏分的综合利用", 《石油化工》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112063102A (en) * | 2020-10-27 | 2020-12-11 | 安徽同心新材料科技有限公司 | Petroleum resin with excellent ageing resistance and preparation method thereof |
| CN113336891A (en) * | 2021-06-22 | 2021-09-03 | 大庆华科股份有限公司 | Methyl styrene and indene modified dicyclopentadiene petroleum resin and preparation method thereof |
| CN113461859A (en) * | 2021-07-02 | 2021-10-01 | 青岛海伊诺新材料科技有限公司 | Preparation method of light-colored cold-polymerized C5/C9 copolymerized petroleum resin |
| CN113461859B (en) * | 2021-07-02 | 2023-10-20 | 青岛海伊诺新材料科技有限公司 | Preparation method of light-colored cold-polymerized C5/C9 copolymerized petroleum resin |
| CN114395077A (en) * | 2021-12-28 | 2022-04-26 | 恒河材料科技股份有限公司 | Preparation method of naphthenic filling oil |
| CN114395077B (en) * | 2021-12-28 | 2024-02-09 | 恒河材料科技股份有限公司 | Preparation method of cycloalkyl filling oil |
| CN114573752A (en) * | 2022-03-11 | 2022-06-03 | 广东新华粤石化集团股份公司 | Modified petroleum resin with narrow molecular weight distribution, preparation method and application |
| CN114573752B (en) * | 2022-03-11 | 2023-11-03 | 广东新华粤石化集团股份公司 | Modified petroleum resin with narrow molecular weight distribution, preparation method and application |
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