CN106590729B - A kind for the treatment of process of softening oil - Google Patents
A kind for the treatment of process of softening oil Download PDFInfo
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- CN106590729B CN106590729B CN201710087675.8A CN201710087675A CN106590729B CN 106590729 B CN106590729 B CN 106590729B CN 201710087675 A CN201710087675 A CN 201710087675A CN 106590729 B CN106590729 B CN 106590729B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
- C10G29/20—Organic compounds not containing metal atoms
- C10G29/22—Organic compounds not containing metal atoms containing oxygen as the only hetero atom
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4006—Temperature
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to a kind for the treatment of process of softening oil, preparation method includes the following steps：By the byproduct residual oil or heavy oil after Petroleum refining, the crosslinking agent and catalyst of feedstock oil certain mass is added, under the conditions of nitrogen protection; heating stirring is uniform; after milled processed, squeezes into micro passage reaction through mass flow pump and be modified reaction, obtain modified oil product.Method equipment requirement according to the present invention is simple, oil product treatment process is rapidly and efficiently, gained oil product is a kind of softening agent of function admirable, polycyclic aromatic content is low in modified oil product, Product environment close friend is pollution-free, it applies in rubber, glue bond can be effectively improved, there is preferable economic benefit.
Description
Technical field
The present invention relates to a kind for the treatment of process of softening oil, belong to chemical products field, and product is mainly used in rubber system
In product such as tire industry.
Background technology
Residual oil or heavy oil are the remaining mink cell focuses after crude oil extraction gasoline, diesel oil, and basic unit is low molecular monocycle
Aromatic hydrocarbons, polycyclic aromatic hydrocarbon (polycyclic aromatic hydrocarbons, abbreviation PAHs) and polycyclic aromatic hydrocarbon.And 4-6
The polycyclic aromatic hydrocarbons (PAH) of ring has strong carcinogenicity, and most representative is 3,4- BaPs (BaP).Its mechanism of carcinogenesis is polycyclic
Aromatic hydrocarbon enters internal, and various intermediate products and final product are generated with function oxidase metabolism, and some of metabolites can be with
DNA covalent bonds form PAH-DNA adducts, and DNA damage, induced gene mutation or even induced tumor is caused to be formed.For this purpose,
The western countries such as Germany and Poland have had been switched off most of softening oil processing factories, while providing polycyclic aromatic hydrocarbons (PAH) in softening oil product
Content is less than 50mg/kg, and the application which limits oil product in many fields, China is also in developing country, rubber product
Equal fields are also quite big to the dependence of rubber softening oil and demand, how to effectively reduce polycyclic aromatic hydrocarbon content in oil product, subtract
Few environmental pollution becomes the important topic of current research.
The method for reducing polycyclic aromatic hydrocarbon in the softening oil product such as residual oil or heavy oil at present mainly has Ozonation, vacuum distillation
Method, ultraviolet irradiation, low boiling point solvent extract method and chemic modified method etc., most economical most convenient is most expected in these methods
Realize that industrialized is exactly chemical modification, according to similar compatibility principle, the crosslinking agent of selection should dissolve each other with polycyclic aromatic hydrocarbon in oil product,
Contain active group (such as electron-donating group) simultaneously.
Crosslinking agents and the heavy oil such as chemic modified method generally use polyethylene glycol, polystyrene, furan resin, paraformaldehyde or
Polycyclic aromatic hydrocarbons (PAH) reaction (PAHs) in residual oil, generates condensation polycyclic aromatic hydrocarbon resin.But heavy oil or residual oil ingredient are more multiple
It is miscellaneous, along with polycyclic aromatic hydrocarbons (PAH) reactivity differs and crosslinking agent factors such as dissolubility in oil product so that the extent of reaction
Low, the detoxification treatment of polycyclic aromatic hydrocarbons (PAH) (PAHs) is ineffective.
Based on previous karyotype studies, present invention seek to address that chemic modified method polycyclic aromatic hydrocarbons (PAH) (PAHs) detoxification treatment is low,
The extent of reaction is low, and gained softening oil leads to problems such as performance poor because inhomogenous in mixed process.The present invention is proposed using micro-
Channel reactor is as reaction vessel, to solve the above problems.Micro passage reaction is size between 10 to 300 microns
A kind of duct type microreactor continuously flowed, microreactor have great specific surface area, up to stirred tank specific surface area
Even thousands of times of hundred times, the basic advantage thus brought is great heat exchange efficiency and mixing efficiency, can be accurately controlled anti-
It answers temperature and reaction mass by the instantaneous mixing of accurate proportioning, greatly improves reaction efficiency.Exactly these features so that in microchannel
Reactor plays good effect in terms of handling polycyclic aromatic hydrocarbons (PAH) (PAHs) detoxification, the extent of reaction is greatly improved, to have
Effect solves the problems such as detoxification efficiency is low, and the extent of reaction is low, and oil product mixing is inhomogenous.
Invention content
The present invention relates to a kind for the treatment of process of softening oil, preparation method includes the following steps：After taking Petroleum refining
The 5-50% crosslinking agents of raw material oil quality and the catalyst of raw material oil quality 1-10% is added, in nitrogen in byproduct residual oil or heavy oil
Under the conditions of gas shielded, it is heated to 70-200 DEG C, is stirred evenly, after milled processed, micro passage reaction is squeezed into through mass flow pump
In, it is heated to 70-200 DEG C, handles 0.5-6h, obtains modified oil product.Method equipment requirement according to the present invention is simple, oil product
Rapidly and efficiently, gained oil product is a kind of softening agent of function admirable to treatment process, and polycyclic aromatic content is low in oil product, product ring
Border close friend is pollution-free, applies in rubber, can effectively improve glue bond, has preferable economic benefit.
The feedstock oil selects byproduct residual oil or heavy oil after taking Petroleum refining.It can be subdivided into according to viscosity and density
The mixing of high viscosity, low-viscosity, big density, small density oil product or above-mentioned four kinds of oil products.
The crosslinking agent, it is characterised in that：Crosslinking agent selects polyethylene glycol, polystyrene, furane resins, polyethylene tree
Fat, 5 resin of carbon, aldehydes, aromatic alcohol, aromatic aldehydes and the above compound derivative or above-mentioned crosslinking agent mixing.
The catalyst, it is characterised in that：Catalyst selects sulfuric acid, p-methyl benzenesulfonic acid, P-TOLUENE SULFO ACID 99, nitric acid, salt
The Bronsted acids such as acid；Either select the mixing of the Lewis such as boron chloride, alchlor acid or above-mentioned catalyst.
The micro passage reaction, it is characterised in that：Micro passage reaction use temperature range is -100~400 DEG C,
Pipe diameter is 10~1000 microns.
Contain the higher polycyclic aromatic hydrocarbons (PAH) of concentration in oil product selected by the present invention, usual content is in 35-55%, in order to handle
Fall the polycyclic aromatic hydrocarbon in oil product, obtains a kind of environmentally friendly, rubber softening oil of good performance, add polyethylene glycol, paraformaldehyde
Crosslinking agent of the equal polymer as chemical modification, it is heated to be condensed to yield condensation polycyclic aromatic hydrocarbon resin, it changes more in oil product
Aromatic hydrocarbon ring structure, reduces it to environmental hazard toxicity, while during being used as rubber product softening oil, Ji Nengti
For bating effect, and can play the role of improving sizing material tack.
The reactor that the present invention uses is different from traditional heating stirring kettle, but selects more several than stirred tank specific surface area
Hundred times even thousands of times of micro passage reaction, great heat exchange efficiency and mixing efficiency, can accurately control reaction temperature
With reaction mass by the instantaneous mixing of accurate proportioning, reaction efficiency and speed are greatly improved, obtains the high modified softening of the extent of reaction
Oil, avoid in reaction process because steric effect, material composition is complicated, reaction is insufficient the problems such as occur, reduce the reaction used time
To reduce production cost.
The technique that the application proposes has following advantageous effect：
Advantageous effect
A kind for the treatment of process of softening oil according to the present invention, the advantage is that：
(1) equipment requirement is simple, and process characteristic is suitble to heavy industrialization, consecutive production.
(2) raw material needed for is simple and easy to get, and simple for process easy to operate, reaction time consumption is short, and modification is of low cost, and modification efficiency is high.
(3) production technology involved by is safe, and product detoxification efficiency is good, environmental-friendly, three-waste free discharge.
(4) product yield is high, and gained softening oil mass uniformity is good.
(5) this product is good using bating effect in rubber product, can be uniformly distributed in sizing material, be effectively improved sizing material
Processing performance.
(6) product comprehensive performance protrudes, and improves the tack of sizing material, the adhesiveness of steel wire and rubber when improving manufacture tire
Can, assign the good comprehensive performance of rubber product.
(7) this product is modified at low cost, and product quality stability is high, and the market competitiveness is strong, with good economic efficiency,
Social benefit.
Specific implementation mode
Embodiment 1
It takes the by-product heavy oil after 100kg Petroleum refinings to pour into heating reaction kettle, is added 5kg polyethylene glycol, 1kg sulfuric acid,
It is passed through nitrogen, 70 DEG C is heated to, stirs evenly, after crossing 100nm sieves, size is squeezed into through mass flow pump for milled processed
In 1000nm micro passage reactions, 70 DEG C, modified-reaction 0.5h are heated to, obtains modified oil product.Modified oil product is carried out polycyclic
18 detections of aromatic hydrocarbon (PAHs), bond properties detection formula：Smoke sheet rubber 100pr, zinc oxide 8pr, accelerator DZ 1.25pr,
Carbon black N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr carry out the physical property detection of rubber according to national standards.
Embodiment 2
It takes the byproduct residual oil after 100kg Petroleum refinings to pour into heating reaction kettle, is added 50k metaformaldehydes, 10kg sulfuric acid,
It is passed through nitrogen, 200 DEG C is heated to, stirs evenly, after crossing 100nm sieves, size 50nm is squeezed into through mass flow pump for milled processed
Micro passage reaction in, be heated to 200 DEG C, modified-reaction 6h, obtain modified oil product.Polycyclic aromatic hydrocarbons (PAH) is carried out to modified oil product
(PAHs) 18 detections, bond properties detection formula：Smoke sheet rubber 100pr, zinc oxide 8pr, accelerator DZ 1.25pr, carbon black
N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr carry out the physical property detection of rubber according to national standards.
Embodiment 3
It takes the byproduct residual oil after 100kg Petroleum refinings to pour into heating reaction kettle, 20kg polystyrene is added, 2kg is to first
Base benzene sulfonic acid, is passed through nitrogen, is heated to 100 DEG C, stirs evenly, milled processed, after crossing 100nm sieves, is beaten through mass flow pump
In the micro passage reaction for entering size 100nm, 150 DEG C, modified-reaction 2h are heated to, obtains modified oil product.To modified oil product into
18 detections of row polycyclic aromatic hydrocarbons (PAH) (PAHs), bond properties detection formula：Smoke sheet rubber 100pr, zinc oxide 8pr, accelerator DZ
1.25pr, carbon black N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr carry out the object of rubber according to national standards
Property detection.
Embodiment 4
It takes the byproduct residual oil after 100kg Petroleum refinings to pour into heating reaction kettle, 30kg formaldehyde is added, 3kg is to methylbenzene
Sulfonic acid is passed through nitrogen, is heated to 90 DEG C, stirs evenly, milled processed, and after crossing 100nm sieves, size is squeezed into through mass flow pump
In the micro passage reaction of 10nm, 100 DEG C, modified-reaction 1h are heated to, obtains modified oil product.Polycyclic virtue is carried out to modified oil product
18 detections of fragrant hydrocarbon (PAHs) carry out the physical property detection of rubber according to national standards.
Embodiment 5
It takes the by-product heavy oil after 100kg Petroleum refinings to pour into heating reaction kettle, 40kg terephthalyl alcohols, 3kg tri- is added
Aluminium chloride is passed through nitrogen, is heated to 140 DEG C, stirs evenly, milled processed, after crossing 100nm sieves, is squeezed into through mass flow pump
In the micro passage reaction of size 80nm, 180 DEG C, modified-reaction 6h are heated to, obtains modified oil product.Modified oil product is carried out more
18 detections of aromatic hydrocarbon ring (PAHs), bond properties detection formula：Smoke sheet rubber 100pr, zinc oxide 8pr, accelerator DZ
1.25pr, carbon black N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr carry out the object of rubber according to national standards
Property detection.
Embodiment 6
It takes the byproduct residual oil after 100kg Petroleum refinings to pour into heating reaction kettle, is added 25kg paraformaldehydes, 2kg sulfuric acid,
It is passed through nitrogen, 110 DEG C is heated to, stirs evenly, after crossing 100nm sieves, size is squeezed into through mass flow pump for milled processed
In the micro passage reaction of 300nm, 180 DEG C, modified-reaction 4h are heated to, obtains modified oil product.Modified oil product is carried out polycyclic
18 detections of aromatic hydrocarbon (PAHs), bond properties detection formula：Smoke sheet rubber 100pr, zinc oxide 8pr, accelerator DZ 1.25pr,
Carbon black N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr carry out the physical property detection of rubber according to national standards.
Embodiment 7
It takes the byproduct residual oil after 100kg Petroleum refinings to pour into heating reaction kettle, 20kg terephthalyl alcohols and 10kg is added
Polyethylene glycol, 2kg sulfuric acid and 2kg alchlors, are passed through nitrogen, are heated to 120 DEG C, stir evenly, milled processed, cross 100nm
After sieve, is squeezed into the micro passage reaction of size 500nm through mass flow pump, be heated to 160 DEG C, modified-reaction 5h is obtained
Modified oil product.18 detections of polycyclic aromatic hydrocarbons (PAH) (PAHs), bond properties detection formula are carried out to modified oil product：Smoke sheet rubber 100pr,
Zinc oxide 8pr, accelerator DZ 1.25pr, carbon black N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr, according to state
Family's standard carries out the physical property detection of rubber.
Embodiment 8
It takes the by-product heavy oil after 100kg Petroleum refinings to pour into heating reaction kettle, 10kg metaformaldehydes and 10kg pairs is added
Benzene dimethanol, 1kg p-methyl benzenesulfonic acids and 1kg nitric acid, are passed through nitrogen, are heated to 105 DEG C, stir evenly, milled processed, mistake
After 100nm sieves, is squeezed into the micro passage reaction of size 800nm through mass flow pump, is heated to 150 DEG C, modified-reaction 3h,
Obtain modified oil product.18 detections of polycyclic aromatic hydrocarbons (PAH) (PAHs), bond properties detection formula are carried out to modified oil product：Smoke sheet rubber
100pr, zinc oxide 8pr, accelerator DZ 1.25pr, carbon black N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr,
The physical property detection of rubber is carried out according to national standards.
Embodiment 9
It takes the by-product heavy oil after 100kg Petroleum refinings to pour into heating reaction kettle, 28kg polyvinyl resins, 3kg sulphur is added
Acid is passed through nitrogen, is heated to 150 DEG C, stirs evenly, milled processed, and after crossing 100nm sieves, size is squeezed into through mass flow pump
In the micro passage reaction of 250nm, 190 DEG C, modified-reaction 4h are heated to, obtains modified oil product.Modified oil product is carried out polycyclic
18 detections of aromatic hydrocarbon (PAHs), bond properties detection formula：Smoke sheet rubber 100pr, zinc oxide 8pr, accelerator DZ 1.25pr,
Carbon black N330 55pr, insoluble sulfuy 4.4pr, antioxidant 4020 2pr carry out the physical property detection of rubber according to national standards.
Embodiment 10
It takes the byproduct residual oil after 100kg Petroleum refinings to pour into heating reaction kettle, 15kg furane resins is added, 2kg is to first
Base benzene sulfonic acid, is passed through nitrogen, is heated to 200 DEG C, stirs evenly, milled processed, after crossing 100nm sieves, is beaten through mass flow pump
In the micro passage reaction for entering size 100nm, 200 DEG C, modified-reaction 1h are heated to, obtains modified oil product.To modified oil product into
18 detections of row polycyclic aromatic hydrocarbons (PAH) (PAHs) carry out the physical property detection of rubber according to national standards.
Comparative example 1：
The byproduct residual oil after Petroleum refining or heavy oil are taken, 18 detections of polycyclic aromatic hydrocarbons (PAH) (PAHs) are carried out to oil product, are glued
Close performance detection formula：Smoke sheet rubber 100pr, zinc oxide 8pr, accelerator DZ 1.25pr, carbon black N330 55pr, insoluble sulfuy
4.4pr, antioxidant 4020 2pr carry out the physical property detection of rubber according to national standards.
Softening oil applies the physical property testing result in rubber product in table 1, embodiment
Claims (4)
1. a kind for the treatment of process of softening oil, it is characterised in that：The byproduct residual oil after Petroleum refining or heavy oil is taken to pour into heating
5~50% crosslinking agents of raw material oil quality and the catalyst of raw material oil quality 1~10% is added, in nitrogen protection item in stirred tank
Under part, heating stirring kettle is heated to 70~200 DEG C, is stirred evenly, milled processed, after crossing 100nm sieves, pumped through mass flow
Micro passage reaction is squeezed into, is heated to 70~200 DEG C, handles 0.5~6h, obtains modified oil product.
2. a kind for the treatment of process of softening oil according to claim 1, it is characterised in that：Crosslinking agent selects polyethylene tree
Fat, 5 resin of carbon, polyethylene glycol, polystyrene, furane resins, aldehydes, aromatic alcohol, aromatic aldehydes or more compound are spread out
The mixing of biology or above-mentioned crosslinking agent.
3. a kind for the treatment of process of softening oil according to claim 1, it is characterised in that：Catalyst selects sulfuric acid, to first
Base benzene sulfonic acid, toluenesulfonic acid, nitric acid, hydrochloric acid；Either select the mixing of boron chloride, alchlor or above-mentioned catalyst.
4. a kind for the treatment of process of softening oil according to claim 1, it is characterised in that：Micro passage reaction temperature in use
Ranging from -100~400 DEG C, pipe diameter is 10~1000 microns.
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| CN201710087675.8A CN106590729B (en) | 2017-02-18 | 2017-02-18 | A kind for the treatment of process of softening oil |
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| CN111635778A (en) * | 2020-06-22 | 2020-09-08 | 中海沥青股份有限公司 | Rubber plasticizer for petroleum-based environment-friendly reclaimed rubber and preparation method thereof |
| CN112063186A (en) * | 2020-09-14 | 2020-12-11 | 江苏麒祥高新材料有限公司 | Preparation method of environment-friendly rubber oil and prepared environment-friendly rubber oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1626559A (en) * | 2003-12-09 | 2005-06-15 | 中国石油化工股份有限公司九江分公司 | New method for separating reaction of catalyzing oil slurry |
| CN103756708A (en) * | 2014-01-16 | 2014-04-30 | 神华集团有限责任公司 | Modified asphalt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9752098B2 (en) * | 2012-08-13 | 2017-09-05 | Research Institute Of Highway, Ministry Of Transportation | Bio-asphalt, bio-asphalt composition and method for preparing them |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1626559A (en) * | 2003-12-09 | 2005-06-15 | 中国石油化工股份有限公司九江分公司 | New method for separating reaction of catalyzing oil slurry |
| CN103756708A (en) * | 2014-01-16 | 2014-04-30 | 神华集团有限责任公司 | Modified asphalt and preparation method thereof |
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Address after: 236000 Yingzhou District, Fuyang City, Anhui Province Patentee after: New Anhui Mstar Technology Ltd Address before: 236000 Xin'an Avenue 518, Fuyang Economic and Technological Development Zone, Fuyang City, Anhui Province Patentee before: New Anhui Mstar Technology Ltd |