CN101684185A - Production method of high-aromatic-hydrocarbon environment-friendly rubber oil - Google Patents
Production method of high-aromatic-hydrocarbon environment-friendly rubber oil Download PDFInfo
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Abstract
The invention relates to a production method of high aromatic hydrocarbon environment-friendly rubber oil, which takes heavy solvent extract oil of a lubricating oil solvent refining device as a raw material; adding an auxiliary agent into the raw materials, and then refining the solvent; the heavy solvent extract oil has a flash point of more than 200 ℃ and a kinematic viscosity of more than 15.0mm at 100 DEG C2(s) a CA value of greater than 35.0%; the auxiliary agent is simple substance hydrocarbon or light hydrocarbon oil with small density, small viscosity and boiling point in the range of 80-300 ℃; the solvent is N-methyl pyrrolidone, phenol or furfural; the temperature of the top of the refining tower is 50-100 ℃, the temperature of the bottom of the refining tower is 30-100 ℃, and the mass ratio of the raw materials, the auxiliary agent and the solvent is as follows: 1.0: 0.1-0.5: 2.0-5.0; the refined oil has high aromatic hydrocarbon content, the CA value is more than 19.0 percent, the aromatic hydrocarbon content is more than 50.0 percent, the PCA content measured by an IP346 method is less than 3.0 percent, benzopyrene is less than 1PPM, and the total content of 8 specific polycyclic aromatic hydrocarbons is less than 10 PPM.
Description
Technical field
The present invention relates to a kind of production method of the high-arene environment-friendly rubber oil that meets the European Union environmental protection standard-required of rubber industry use.
Background technology
Aromatic hydrocarbon rubber oil is called for short aromatic hydrocarbon oil, it is the widely used a kind of processing aid of rubber and tire production industry, mainly in order to improve the dispersiveness of other Synergist S-421 95 in the sizing material processing, improve flexibility, plasticity and calendering, the extrusion performance of sizing material, save the power consumption when mixing, can improve simultaneously the physical and mechanical properties of sizing material, reduce production costs.Aromatic hydrocarbon oil generally by the byproduct of lubricating oil solvent device-extract oily direct production out, requires to have higher aromaticity content on product index.But along with in the world wide to the concern of environmental issue and going deep into to the petroleum chemicals toxicity research, contain carinogenicity polycyclic aromatic hydrocarbons such as benzopyrene in the aromatic hydrocarbon oil, in oil-filled glue and tire production, use, can the problem that human body and environment produce toxic have been studies confirm that, for this reason, 2005/69/EC environmental protection instruction signed and issued by European Parliament and EU Council the end of the year 2005.This instruction has proposed and will eliminate at rubber and tyre production enterprise on January 1st, 2010 time limit of aromatic hydrocarbon oil comprehensively, and the environmental protection index of the rubber oil that oil-filled glue and tyre industry are used formulates the following rules: 1. the content of the PCA that measures according to the IP346 method must be less than 3%, 2. benzopyrene content less than 1PPM 3. the total content of 8 kinds of specific polycyclic aromatic hydrocarbonss less than 10PPM.Feature of environmental protection detected result to the aromatic hydrocarbon oil of domestic present production shows, its PCA content is generally about 20% or bigger, be not more than 3% environmental protection index requirement head and shoulders above, rubber and tire production industry can not have been continued to be applied to, though and the naphthenic oil PCA content that is used for light oil-filled glue and rubber item production can satisfy the environmental protection index requirement, but its aromaticity content is low, can not satisfy the technical requirements aspect rubber compatibility.Therefore, the environment-friendly rubber oil that have higher aromaticity content, satisfies the European Union environmental protection index request is demanded exploitation urgently.It is a kind of so that to extract oil out be raw material production PCA less than the production technique of 3% environment-friendly rubber oil that European patent EP 1106673B1 provides, its operational path of taking is solvent pre-refining-hydrofining, the solvent that uses in the solvent pre-refining stage is NMP, taked to add therein a certain proportion of water improves extraction rate was acquired as auxiliary agent method, but for guaranteeing certain yield, the solvent treatment step can only be reduced to 9.0-15.0% with the PCA that extracts oil out, to treated oil be reached and be not less than 3.0% environmental protection index requirement, and other two indexs that above-mentioned European Union environmental protection instruction is mentioned are not mentioned, and whole explained hereafter investment is bigger, and process cost is higher.
Though solvent treatment is widely used a kind of maturation process in the refined course of lubricating oil, the means of introducing auxiliary agent also see in domestic and international many patents and the report, but the auxiliary agent that uses generally is to add in the solvent, extractive raw material is a lubricating oil distillate, and purpose is to improve the yield of lubricant base.Some also only are that stable hydrocarbon, raising lubricant base yield or the production catalytically cracked material of extracting out in the oil with recovery is purpose about extracting the oily patent of utilizing out, and do not relate to extracting the direct extracting of oil out.
Summary of the invention
The heavy solvent that the objective of the invention is to rely on domestic resource selection lube oil finishing device to produce is extracted the oily raw material that is out, by in raw material, adding auxiliary agent and suitable refining solvent, on the extraction plant raw material is being carried out the multi-stage countercurrent extracting continuously, optionally remove poisonous polycyclic aromatic hydrocarbons in the furfural extract oil, keep nontoxic aromatic hydrocarbons, when guaranteeing that treated oil satisfies the environmental protection index requirement, keep higher aromaticity content, thereby realize the production purpose of high-arene environment-friendly rubber oil.
The invention is characterized in: extracting oil out with the heavy solvent of lubricating oil solvent device is raw material, adds auxiliary agent in raw material, carries out solvent treatment again; The mass ratio of raw material, auxiliary agent, solvent is: 1.0: 0.1～0.5: 2.0～5.0.
Heavy solvent is extracted oil out, and its flash-point is greater than 200 ℃, and 100 ℃ of kinematic viscosity are greater than 15.0mm
2/ s, the CA value is greater than 35.0%;
Auxiliary agent is that density is little, viscosity is little, boiling point is in the simple substance hydrocarbon or the mixes light hydrocarbons of 80-300 ℃ of scope, can realize recycling by solvent recovering system;
Solvent is N-Methyl pyrrolidone, phenol or furfural;
Purification condition is: tower top temperature 50-100 ℃, and column bottom temperature 30-100 ℃, agent-oil ratio 0.5-5.0.
Extracting oil out with the heavy solvent of lube oil finishing device production is raw material, introducing density is little in raw material, viscosity is little, simple substance hydrocarbon or the light hydrocarbons auxiliary agent of boiling point in 80 ℃ of-300 ℃ of scopes, reduce the density difference of viscosity, increase raw material and the solvent of raw material, improve choice of Solvent, thereby realize the selectivity of raw material refining, manufactured experimently out that aromatic carbon content is not less than 19.0%, aromaticity content is greater than 50.0%, every environmental protection index satisfies the environment-friendly rubber oil that European Union environmental protection requires.Whole technology simple economy.
The effect of invention
The PCA content that the aromatic hydrocarbon oil of refinement treatment of the present invention is measured with the IP346 method less than 3.0%, benzopyrene less than 1PPM, 8 kinds of specific polycyclic aromatic hydrocarbons total contents less than 10PPM, reach the environmental protection index requirement of European Union environmental protection instruction 2005/69/EC fully, and the aromaticity content height of treated oil, the CA value more than 19.0%, aromaticity content is greater than 50.0%, investigate by effect, satisfy the technical requirement of tyre industry fully environment-friendly rubber oil at the tyres for passenger cars tread rubber.Applicating evaluating at the tyres for passenger cars tread rubber the results are shown in Table 5-table 7.The process for refining of the high-arene environment-friendly rubber oil of the present invention's exploitation need not big technological transformation, only need before raw material advances extraction tower, to increase the mixing tank of a raw material and auxiliary agent, the storage tank and separating tank transformed of the solvent recovering system of former solvent treatment technology got final product.Adopting this process for refining, is that the mass yield of the treated oil of raw material production can reach more than 50% with the paraffinic base furfural extract oil, and the CA value is greater than 21.0%; The mass yield of treated oil that with cycloalkyl heavy grease furfural extract oil is raw material production is more than 30%, and the CA value is not less than 19.0%.
Description of drawings
The technological process of production synoptic diagram of Fig. 1 high-arene environment-friendly rubber oil.
Wherein: 1-mixing tank, 2-extraction tower, 3-raffinate stripping tower, 4-Extract flashing tower, 5-extract stripper, 6-dehydration tower, 7-separated from solvent jar.
Embodiment
Raw material and auxiliary agent are after mixing tank 1 is mixed in proportion, enter extraction tower 2, solvent is advanced on extraction tower 2 tops, raw material and auxiliary agent extraction tower 2 carry out extracting refining after, after raffinate flows out from extraction tower 2 tops, enter raffinate stripping tower 3 and remove auxiliary agent and solvent, remove raffinating oil behind auxiliary agent and the solvent and be high-arene environment-friendly rubber oil; The effusive auxiliary agent in raffinate stripping tower 3 tops enters separated from solvent jar 7 with solvent after condensation separates; Successively enter Extract flashing tower 4 and extract stripper 5 removes auxiliary agent and solvent from the effusive Extract in extraction tower 2 bottoms, auxiliary agent that removes and solvent also enter separated from solvent jar 7 after condensation; Extract stripper 5 bottoms are effusive to be the extraction oil of deviating from solvent and auxiliary agent; The layering of solvent in the separated from solvent jar 7 owing to the density difference, the upper strata is an auxiliary agent, and lower floor is a solvent, and the centre is a water layer; The aqueous solution in the separated from solvent jar 7 further removes solvent through dehydration tower 6, and auxiliary agent in the separated from solvent jar 7 and solvent cycle are used.
With Dalian Qi Chang produce to subtract four line paraffinic base furfural extract oils be raw material, on laboratory pilot scale extraction plant, with the boiling range scope is that 180 ℃-300 ℃ light hydrocarbon is an auxiliary agent, with the furfural is refining solvent, under the purification condition of agent-oil ratio 2.0-4.0 (mass ratio), tower top temperature 50-80 ℃, column bottom temperature 30-50 ℃, obtained yield and reached 56.8%, the CA value is 22.8%, PCA is 2.6% high-arene environment-friendly rubber oil.
Subtracting three-way cycloalkyl furfural extract oil with the Liaohe River is raw material, on laboratory pilot scale extraction plant, with the boiling range scope is that 180 ℃-300 ℃ light hydrocarbon is an auxiliary agent, with the furfural is refining solvent, under the purification condition of agent-oil ratio 2.0-4.0 (mass ratio), tower top temperature 50-80 ℃, column bottom temperature 30-50 ℃, obtained yield and reached 35.0%, the CA value is 19.4%, PCA is 2.3% high-arene environment-friendly rubber oil.
With Dalian Qi Chang produce to subtract four line paraffinic base furfural extract oils be raw material, on laboratory pilot scale extraction plant, with a kind of simple substance hydrocarbon of boiling point about 130 ℃ is auxiliary agent, with the furfural is refining solvent, under the purification condition of agent-oil ratio 2.0-4.0 (mass ratio), tower top temperature 50-80 ℃, column bottom temperature 30-50 ℃, obtained yield and reached 56.0%, the CA value is 25.0%, PCA is 2.5% high-arene environment-friendly rubber oil.
Subtracting three-way cycloalkyl furfural extract oil with the Liaohe River is raw material, on laboratory pilot scale extraction plant, with a kind of simple substance hydrocarbon of boiling point about 130 ℃ is auxiliary agent, with the furfural is refining solvent, under the purification condition of agent-oil ratio 2.0-4.0 (mass ratio), tower top temperature 50-80 ℃, column bottom temperature 30-50 ℃, obtained yield and reached 33.0%, the CA value is 20.0%, PCA is 2.6% high-arene environment-friendly rubber oil.
The character that embodiment 1 and 3 used experimental raw-Dalian Qi Chang subtract four line furfural extract oils sees Table 1, adopts two kinds of auxiliary agents respectively, is that two kinds of refining oil propertiess that solvent treatment obtains see Table 2 with the furfural.
Table 1 Dalian Qi Chang subtracts four line paraffinic base furfural extract oil physico-chemical properties
| Project | Analytical results |
| Density (20 ℃)/Kg.m -3 | ??990.6 |
| Kinematic viscosity/mm 2.s -1??40℃ ??100℃ | ? ??1876.8 ??30.7 |
| Flash-point (opening) ℃ | ??258 |
| Refractive index N D 20 | ??1.5664 |
| Refractivity intercept RI | ??1.0711 |
| Viscosity gravity constant VGC | ??0.9255 |
| PONA analysis/% C A??C N??C P??PCA％ | ? ??40.0 ??17.5 ??42.5 ??17.16 |
Table 2 Dalian Qi Chang subtracts four line furfural extract oil furfural treatment oil propertiess
| |
1# (auxiliary agent is the simple substance hydrocarbon) | 2# (auxiliary agent is a light hydrocarbon) |
| The treated oil yield, Wt% | ??56.0.0 | ??56.8 |
| Density (20 ℃)/Kg.m -3 | ??950.1 | ??941.8 |
| Kinematic viscosity/mm 2.s -1??100℃ | ? ??17.28 | ? ??16.87 |
| Refractive index N D 20 | ??1.5304 | ??1.5250 |
| Refractivity intercept RI | ??1.05535 | ??1.0541 |
| Viscosity gravity constant VGC | ??0.8856 | ??0.8755 |
| PONA analysis/% C A??C N??C PThe PCA% benzopyrene, the specific 8 kinds of polycyclic aromatic hydrocarbon contents of μ g/g, μ g/g | 25.4 29.4 45.2 2.48 fail to measure 1.3 | 22.8 28.6 48.6 2.6 fail to measure 1.6 |
The character that embodiment 2 and 4 used experimental raw-Liaohe River petrochemical industry subtract three-way furfural extract oil sees Table 3, adopts two kinds of auxiliary agents respectively, is that two kinds of refining oil propertiess that solvent treatment obtains see Table 4 with the furfural.
Table 3 Liaohe River subtracts the character of three-way cycloalkyl furfural extract oil
| Project | Analytical results |
| Density (20 ℃)/kg.m -3 | ??1018.4 |
| Kinematic viscosity/mm 2.s -1??100℃ | ? ??39.22 |
| Flash-point (opening)/℃ | ??236 |
| Zero pour/℃ | ??18 |
| Sulphur content/μ g/g -1 | ??3743.6 |
| Nitrogen content/μ g/g -1 | ??5623.7 |
| Refractive index N D 20 | ??1.5691 |
| ??VGC | ??0.9574 |
| Carbon type analysis/% C A??C N??C P | ? ??40.0 ??39.0 ??21.0 |
| ??PCA，％ | ??26.2 |
Table 4 Liaohe River subtracts the furfural extracting result of three-way cycloalkyl furfural extract oil
| |
1# (auxiliary agent is a light hydrocarbon) | 2# (auxiliary agent is the simple substance hydrocarbon) |
| The treated oil yield, Wt% | ??35.0 | ??33.0 |
| Density (20 ℃)/Kg.m -3 | ??961.5 | ??963.1 |
| Kinematic viscosity/mm 2.s -1??40℃ ??100℃ | ? ??- ??25.2 | ? ? ??25.13 |
| Refractive index N D 20 | ??1.5283 | ??1.5332 |
| Refractivity intercept RI | ??1.04755 | ??1.05165 |
| Viscosity gravity constant VGC | ??0.8916 | ??0.8937 |
| PONA analysis/% C A??C N??C PThe PCA% benzopyrene, the specific 8 kinds of polycyclic aromatic hydrocarbon contents of μ g/g, μ g/g | 19.4 44.8 36.8 2.33 fail to measure and fail to measure | 23.4 38.0 38.6 2.63 fail to measure and fail to measure |
Table 5 Liaohe River environment-friendly rubber oil car tread rubber vulcanizating glue physical performance is investigated the result
Table 6 Liaohe River environment-friendly rubber oil cross-linked rubber heat aging performance is investigated
Table 7 Liaohe River environment-friendly rubber oil cross-linked rubber abrasion resistance and wet-sliding resistant performance are investigated
| Project | Detected result |
| Average abrasion (g/km) | ??0.2348 |
| Average wear resistance ratio | ??101.3 |
| Harsh abrasion (g/km) | ??1.1572 |
| Harsh wear resistance ratio | ??98.5 |
| Lateral force coefficient u | ??0.9144 |
Claims (1)
1. the production method of a high-arene environment-friendly rubber oil is characterized in that: extracting oil out with the heavy solvent of lubricating oil solvent device is raw material, adds auxiliary agent in raw material, carries out solvent treatment again;
Heavy solvent is extracted oil out, and its flash-point is greater than 200 ℃, and 100 ℃ of kinematic viscosity are greater than 15.0mm
2/ s, the CA value is greater than 35.0%;
Auxiliary agent is that density is little, viscosity is little, boiling point is at the simple substance hydrocarbon or the light hydrocarbon of 80-300 ℃ of scope;
Solvent is N-Methyl pyrrolidone, phenol or furfural;
Purification condition is: tower top temperature 50-100 ℃, column bottom temperature 30-100 ℃, the mass ratio of raw material, auxiliary agent, solvent is: 1.0: 0.1～0.5: 2.0～5.0.
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