CN1055675C - Process for regenerating heat conducting oil hydrogenated terphenyl - Google Patents
Process for regenerating heat conducting oil hydrogenated terphenyl Download PDFInfo
- Publication number
- CN1055675C CN1055675C CN97106998A CN97106998A CN1055675C CN 1055675 C CN1055675 C CN 1055675C CN 97106998 A CN97106998 A CN 97106998A CN 97106998 A CN97106998 A CN 97106998A CN 1055675 C CN1055675 C CN 1055675C
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- CN
- China
- Prior art keywords
- hydrogenated terphenyl
- heat conducting
- conducting oil
- acid
- oil hydrogenated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
The present invention relates to a method for regenerating heat conduction oil with hydrogenated terphenyl. In the method, according to the acid value, the pH value of hydrogenated terphenyl is regulated to neutrality by chemical processing with acid and alkali; next, active carbon is added for adsorption, and the fractional distillation is carried out after a dope and coke are removed by press filtration so that a distillation portion in a range of 330 to 420 DEG C is collected as regenerated hydrogenated terphenyl which can be applied to a system. Hydrogenated terphenyl regenerated by the method has the indexes including the carbon residue, the acid value, the viscosity, the flash point and the distillation range all conforming to a standard, so that the conduction oil prepared from the hydrogenated terphenyl is ensured to normally work and equipment is prevented from corrosion and explosion accidents.
Description
The present invention relates to be used as in the chemical industry renovation process of renovation process, particularly heat conducting oil hydrogenated terphenyl of a kind of organic heat carrier of well heater heat-transfer medium.
Thermal oil be in the chemical industry as the organic heat carrier of well heater heat-transfer medium, it by well heater with the heat transferred hot cell.Hydrogenated terphenyl is the thermal barrier that high-temperature liquid-phase is used, and it is the product of terphenyl partial hydrogenation, has Heat stability is good, liquid phase use temperature height, zero pour low (＜-25 ℃), fraction heavy (330 ℃-420 ℃), advantages such as steam forces down, and working pressure was low when liquid phase was used.Be widely used in synthon, synthetic resins, medicine and field of petrochemical industry.Hydrogenated terphenyl is operation at high temperature for a long time, can produce thermo-cracking, polycondensation and coking process, and cracking produces low boil component and the high component of boiling, cause flash-point to descend, carbon residue and acid number increase, and blast easily, etching apparatus, long-pending Jiao etc., influence the normal operation of equipment.Therefore hydrogenated terphenyl must be changed or manipulation of regeneration in good time.Adopt simple fractionation process at present, owing to some azeotrope is difficult to remove, thereby hydrogenated terphenyl carbon residue and acid number after handling still can not reach requirement.
The renovation process that the purpose of this invention is to provide a kind of heat conducting oil hydrogenated terphenyl, it all meets the requirements carbon residue, acid number, viscosity, flash-point, boiling range after the hydrogenated terphenyl regeneration, and thermal barrier and equipment can normally be moved, and ensures safety in production.
Method of the present invention follows these steps to: 1. chemical treatment: waste and old heat conducting oil hydrogenated terphenyl is heated to 70-80 ℃, adjusts the pH value to neutral according to acid number adding alkali or acid, wash 2-3 time with clear water; 2. adsorption filtration: the 3-5% by the waste and old hydrogenated terphenyl gross weight after the above-mentioned processing adds gac, is heated to 110-125 ℃, mixes, and the material that is not adsorbed is collected in press filtration while hot; 3. fractionation is refining: above-mentioned material is dropped into the fractionation still, fractionation removes＜the boil high boiling fraction of fraction and＞420 ℃ of 330 ℃ low, collecting 330 ℃ of-420 ℃ of fractions stores into pan tank, utilize again as thermal barrier for system, above-mentioned said alkali can use soda ash or sodium hydroxide, and said acid can be dilute sulphuric acid.
The present invention removes unsaturated materials by chemical treatment, and acid number is descended, high boiling point dope and coke are removed in adsorption filtration, with the hydrogenated terphenyl thermal oil after present method regeneration, each index of its carbon residue, acid number, viscosity, flash-point and boiling range all meets the standard that domestic relevant department formulates, guarantee that the thermal oil diphenyl mixture normally moves, avoid equipment generation burn into blast or influence accidents such as system condition and device damage because of sedimentation of coke.
Hydrogenated terphenyl regeneration embodiment:
With waste and old hydrogenated terphenyl 1500kg, analyze regeneration according to the following steps behind its physical and chemical index (seeing Table 1).
(1) chemical treatment
Above-mentioned waste and old hydrogenated terphenyl is heated to 80 ℃, adds 10%NaCl solution 60kg, stirred 30 minutes, left standstill 60 minutes.Lower floor's waste lye is told, and it is 0.012 KOH mg/g that the upper strata oil analysis records acid number, with clear water washing three times, gets neutral solution 1460kg then.
(2) adsorption filtration
Add the 60kg craboraffin in the above-mentioned neutral solution, be warmed to 110-125 ℃ and stirred 30 minutes, feed plate-and-frame filter press while hot and carry out press filtration, get filtrate 1405kg, filter residue 115kg is the mud shape waste of high boiling point viscous component, coke and gac.
(3) fractionation is refining
Above-mentioned filtrate is dropped in the fractionation still, heating makes temperature in the kettle reach 60 ℃ to carry out underpressure distillation, vacuum tightness keeps 0.095MPa, when temperature in the kettle reaches 220 ℃, when tower top temperature reaches 190 ℃, there is low-boiling-point substance to distillate, when temperature in the kettle reaches 240 ℃, when tower top temperature 210 was spent, condistillation went out low-boiling-point substance 80kg, and this moment, finished product was collected in cutting, temperature in the kettle continues to rise to 320 ℃, 240 ℃ of tower top temperatures get hydrogenated terphenyl finished product 1230kg, emit residue 73kg in still, loss 27kg, product yield 82%, the physical and chemical testing data of regeneration gained finished product see Table 1, and the contrast before and after regenerating from table 1 is as seen, waste and old hydrogenated terphenyl is after the inventive method regeneration, every physicochemical data all is improved, and meets relative national standards, can be used as thermal oil and utilizes.
The regeneration back faint yellow density of outward appearance brownish black (20 ℃) 1.020g/cm before the physical and chemical testing data items regeneration of table 1 heat conducting oil hydrogenated terphenyl
31.005g/cm
3100 ℃ of 170 ℃ of moisture content of flash-point (opening), 0.05% 0.02% kinematic viscosity (40 ℃) 29mm
2/ s 23mm
2/ s boiling range:
280 ℃ 330 ℃ of initial boiling points
5％ 300℃ 335℃
95% 425 ℃ of 405 ℃ of acid number 0.3 KOH mg/g 0.02 KOH mg/g carbon residues, 0.5% 0.02% zero pour-30 ℃-30 ℃
Claims (3)
1. the renovation process of heat conducting oil hydrogenated terphenyl is characterized in that following these steps to: 1. chemical treatment: waste and old heat conducting oil hydrogenated terphenyl is heated to 70-80 ℃, adjusts the pH value to neutral according to acid number adding alkali or acid, wash 2-3 time with clear water; 2. adsorption filtration: the 3-5% by the waste and old hydrogenated terphenyl gross weight after the above-mentioned processing adds gac, is heated to 110-125 ℃, mixes, and the material that is not adsorbed is collected in press filtration while hot; 3. fractionation is refining: above-mentioned material is dropped into the fractionation still, collect 330 ℃ of-420 ℃ of fractions and be the regeneration hydrogenated terphenyl.
2. according to the renovation process of the heat conducting oil hydrogenated terphenyl of claim 1, it is characterized in that said alkali is soda ash or sodium hydroxide solution.
3. according to the renovation process of the heat conducting oil hydrogenated terphenyl of claim 1, it is characterized in that said acid is dilute sulphuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106998A CN1055675C (en) | 1997-06-17 | 1997-06-17 | Process for regenerating heat conducting oil hydrogenated terphenyl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106998A CN1055675C (en) | 1997-06-17 | 1997-06-17 | Process for regenerating heat conducting oil hydrogenated terphenyl |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1202476A CN1202476A (en) | 1998-12-23 |
| CN1055675C true CN1055675C (en) | 2000-08-23 |
Family
ID=5169193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97106998A Expired - Fee Related CN1055675C (en) | 1997-06-17 | 1997-06-17 | Process for regenerating heat conducting oil hydrogenated terphenyl |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1055675C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179375B (en) * | 2015-05-07 | 2019-02-22 | 中国石油化工股份有限公司 | A kind of catalyst and preparation method for aromatic hydrocarbons Heat Conducting Oil Regeneration and Heat |
| CN111018652A (en) * | 2019-12-15 | 2020-04-17 | 江苏曼拓化学有限公司 | Preparation method of high-purity hydrogenated terphenyl heat conduction oil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0546419A1 (en) * | 1991-12-13 | 1993-06-16 | Bayer Ag | Heat transfer liquid and its preparation |
-
1997
- 1997-06-17 CN CN97106998A patent/CN1055675C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0546419A1 (en) * | 1991-12-13 | 1993-06-16 | Bayer Ag | Heat transfer liquid and its preparation |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1202476A (en) | 1998-12-23 |
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