CN1075487A - Utilize the washing oil residue to produce the method for coumarone indene resin - Google Patents
Utilize the washing oil residue to produce the method for coumarone indene resin Download PDFInfo
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- CN1075487A CN1075487A CN 92110837 CN92110837A CN1075487A CN 1075487 A CN1075487 A CN 1075487A CN 92110837 CN92110837 CN 92110837 CN 92110837 A CN92110837 A CN 92110837A CN 1075487 A CN1075487 A CN 1075487A
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- temperature
- oil residue
- washing oil
- still kettle
- cooling
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- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
A kind of method of utilizing the washing oil residue to produce coumarone indene resin relates to a kind of manufacture method of Rubber Softener.Add steam stripped method by distillation and isolate the heterocyclic arene non-polymer, the ash oontent that carries out the method control material that high low levels is in harmonious proportion by the washing oil residue with different ash oontent is removed mechanical impurity below 1% by the heating and filtering method.Feasible process of the present invention, equipment is simple, and the product yield height is turned waste into wealth, and has remedied the under-supply of natural resources, has reduced the production cost of rubber product.
Description
The present invention relates to a kind of rubber and change the manufacture method of agent, specifically a kind of method of utilizing the washing oil residue to produce coumarone indene resin.
The washing oil residue is a kind of black pitch prill shape material that produces in the pitch coal qi exhaustion benzene regenerating wash oil process, long-term waste disposal as the coke-oven plant, serious environment pollution.The relevant document in China and foreign countries is not found to utilize the washing oil residue to produce the report of coumarone indene resin as yet by retrieval.
The purpose of this invention is to provide a kind of method of utilizing the washing oil residue to produce coumarone indene resin, thereby turn waste into wealth, remedied the under-supply of natural resources, reduced the production cost of rubber product.
Contain a large amount of heterocyclic arene polymkeric substance and non-polymer in the washing oil residue, mainly form, secondly also contain a spot of ash content (0.12～3%) and mechanical impurity, softening temperature lower (20 ℃～45 ℃) by vinylbenzene, indenes, coumarone and homologue thereof.The vaporization temperature of above-mentioned heterocyclic arene non-polymer is 200 ℃～360 ℃, if the simple distillation method that adopts is separated, to cause distillation box inner bottom part material charing coking (more than 300 ℃), therefore, the present invention adopts distillation to add steam stripped method to separate, and to reduce Heating temperature, avoids structure deteriorate, the method control material ash oontent that employing is carried out high low levels blending with the washing oil residue of different ash oontent adopts the heating and filtering method to remove mechanical impurity below 1%.
The present invention is achieved in that earlier and will heats in the washing oil residue input blending groove and concoct ash oontent below 1%, when rising to 80 ℃, temperature discharges sedimentary mechanical impurity by the slag-drip opening of blending trench bottom, the vitriol oil of adding 0.3% carried out polycondensation when temperature was 80 ℃～100 ℃, and stir with 60 rev/mins speed, by the insulation spiral pump material is pumped in the still kettle then and heat, when temperature rises to 180 ℃, feed 3kg/cm by the steam valve on the still kettle
2Steam carry out stripping, start water circulating pump simultaneously with crystallisation by cooling distilled heterocyclic arene gas from still kettle in 20 ℃ the water pump entry water cooling tower, and with 20 ℃/time heat-up rate continue still kettle is heated, sampling analysis when temperature rises to 240 ℃～250 ℃, steam off valve and cooling when recording the material softening temperature and being 83 ℃～85 ℃, baiting valve by still kettle when temperature is reduced to 180 ℃～200 ℃ enters crystallisation by cooling in the crystallizing pan with material, recording the material softening temperature is 85 ℃～87 ℃ broken materials and packing, promptly obtains yield and reaches 70%～90% coumarone indene resin.
Accompanying drawing is technological process of production figure of the present invention.
Feasible process of the present invention, equipment is simple, the product yield height, its quality index sees the following form:
| Project | Quality index | Method of testing |
| Outward appearance | The glossiness curing of black | Range estimation |
| Softening point (ring and ball method) | 80℃～90℃ | YB313 |
| Ash content (%) | ≯1.5 | YB313 |
| Acid-base value (%) | ≯0.05 | YB313 |
| Moisture (%) | ≯0.5 | YB313 |
Embodiment: the washing oil residue with 3000kg is a charging capacity, and its physicochemical data is: 45 ℃ of resin contents 85%, ash content 0.8%, mechanical impurity 0.1%, softening temperature.With in the washing oil residue input blending groove of 3000kg and, when rising to 80 ℃, temperature discharges sedimentary mechanical impurity earlier, 95% of adding 90kg H when temperature is 80 ℃～100 ℃ by the slag-drip opening of blending trench bottom with the serpentine heat exchanger heating
2SO
4Carry out polycondensation, and stirred 30 minutes, by the insulation spiral pump material is pumped into heating in the still kettle (horizontal coal pit stove) then, when temperature rises to 180 ℃, feed 3kg/cm by steam valve with 60/ minute speed
2Steam carry out stripping, start water circulating pump simultaneously with crystallisation by cooling distilled heterocyclic arene gas from still kettle in 20 ℃ the water pump entry water cooling tower, and with 20 ℃/time heat-up rate continue still kettle is heated, sampling analysis when temperature rises to 240 ℃, recording material is softened when a little being 83 ℃ the steam off valve and the burner hearth burning things which may cause a fire disaster is withdrawed from the nature cooling, when temperature is reduced to 180 ℃, open baiting valve material is entered crystallisation by cooling in the crystallizing pan, recording the material softening temperature is that 85 ℃ of broken materials and packing are weighed, and obtains the 2800kg coumarone indene resin.The about 80kg of residue at the bottom of the removing still when temperature of still to be distilled is reduced to normal temperature.The softening temperature of product is that 85 ℃, ash content are 0.86%, potential of hydrogen is 0.03%, moisture is 0.3%.
Claims (1)
- A kind of method of utilizing the washing oil residue to produce coumarone indene resin, it is characterized in that to heat in the washing oil residue input blending groove and concocting ash oontent earlier below 1%, when rising to 80 ℃, temperature gets rid of sedimentary mechanical acrobatics by the slag-drip opening of blending trench bottom, the vitriol oil of adding 0.3% carried out polycondensation when temperature was 80 ℃～100 ℃, and stir with 60 rev/mins speed, by the insulation spiral pump material is pumped in the still kettle then and heat, when temperature rises to 180 ℃, feed 3kg/cm by the steam valve on the still kettle 2Steam carry out stripping, start water circulating pump simultaneously with crystallisation by cooling distilled heterocyclic arene gas from still kettle in 20 ℃ the water pump entry water cooling tower, and with 20 ℃/time heat-up rate continue still kettle is heated, sampling analysis when temperature rises to 240 ℃～250 ℃, steam off valve and cooling when recording the material softening temperature and being 83 ℃～85 ℃, baiting valve by still kettle when temperature is reduced to 180 ℃～200 ℃ enters crystallisation by cooling in the crystallizing pan with material, and recording the material softening temperature is 85 ℃～87 ℃ broken materials and packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92110837 CN1029923C (en) | 1992-09-19 | 1992-09-19 | Method for producing coumarone resin using washing-oil residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92110837 CN1029923C (en) | 1992-09-19 | 1992-09-19 | Method for producing coumarone resin using washing-oil residue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1075487A true CN1075487A (en) | 1993-08-25 |
| CN1029923C CN1029923C (en) | 1995-10-04 |
Family
ID=4945004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92110837 Expired - Fee Related CN1029923C (en) | 1992-09-19 | 1992-09-19 | Method for producing coumarone resin using washing-oil residue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1029923C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001374A (en) * | 2015-06-23 | 2015-10-28 | 濮阳市联众兴业化工有限公司 | Method for preparing coumarone resin |
| CN105542081A (en) * | 2015-12-25 | 2016-05-04 | 李道民 | Modified coumarone petroleum resin and preparation method thereof |
| CN105924579A (en) * | 2016-06-24 | 2016-09-07 | 李道民 | Production method of modified and tackified coumarone indene resin |
| CN114774153A (en) * | 2022-04-22 | 2022-07-22 | 包头钢铁（集团）有限责任公司 | Coal blending coking method using washing oil residue as binder and adding non-caking coal |
-
1992
- 1992-09-19 CN CN 92110837 patent/CN1029923C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001374A (en) * | 2015-06-23 | 2015-10-28 | 濮阳市联众兴业化工有限公司 | Method for preparing coumarone resin |
| CN105001374B (en) * | 2015-06-23 | 2017-10-10 | 濮阳市联众兴业化工有限公司 | A kind of method of coumarone indene resin processed |
| CN105542081A (en) * | 2015-12-25 | 2016-05-04 | 李道民 | Modified coumarone petroleum resin and preparation method thereof |
| CN105924579A (en) * | 2016-06-24 | 2016-09-07 | 李道民 | Production method of modified and tackified coumarone indene resin |
| CN114774153A (en) * | 2022-04-22 | 2022-07-22 | 包头钢铁（集团）有限责任公司 | Coal blending coking method using washing oil residue as binder and adding non-caking coal |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1029923C (en) | 1995-10-04 |
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