CN1465559A - Recycling of waste triethylene glycol - Google Patents
Recycling of waste triethylene glycol Download PDFInfo
- Publication number
- CN1465559A CN1465559A CNA021237794A CN02123779A CN1465559A CN 1465559 A CN1465559 A CN 1465559A CN A021237794 A CNA021237794 A CN A021237794A CN 02123779 A CN02123779 A CN 02123779A CN 1465559 A CN1465559 A CN 1465559A
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- Prior art keywords
- triglycol
- glycol
- recycling
- temperature
- triethylene glycol
- 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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- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000002699 waste material Substances 0.000 title claims abstract description 33
- 238000004064 recycling Methods 0.000 title claims description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004821 distillation Methods 0.000 claims abstract description 19
- 239000003345 natural gas Substances 0.000 claims abstract description 17
- 239000003921 oil Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 25
- 238000009835 boiling Methods 0.000 claims description 15
- 235000009508 confectionery Nutrition 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010586 diagram Methods 0.000 claims description 3
- 229920002521 macromolecule Polymers 0.000 claims description 2
- 238000013475 authorization Methods 0.000 claims 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 6
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 150000001336 alkenes Chemical class 0.000 abstract 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 description 9
- 238000006297 dehydration reaction Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000001172 regenerating effect Effects 0.000 description 7
- 230000003750 conditioning effect Effects 0.000 description 5
- 238000012423 maintenance Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 208000036829 Device dislocation Diseases 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000002354 daily effect Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A method for recovering pure triethylene glycol from waste triethylene glycol solution after purifying natural gas containing impurities such as oil, water, ethylene glycol and the like is characterized in that the waste triethylene glycol solution is recycled, the pressure of the whole system is lower than-0.08 MPa, a temperature-controllable heating system is adopted, when the distillation temperature is 20-180 ℃, first fractions of light substances such as condensate oil, water, ethylene glycol and the like are distilled, when the temperature reaches 180-190 ℃, second fractions of light yellow and transparent triethylene glycol products are distilled, the light yellow and transparent triethylene glycol products do not contain benzene, aromatic hydrocarbon and olefin substances, when the temperature is increased to be more than 200 ℃, the remaining third fractions which are black and have high viscosity are evaporation residues, so that the cost can be greatly saved, and the problems of difficult treatment of taking triethylene glycol as waste and possible environmental pollution can be solved.
Description
Affiliated field
The invention belongs to chemical field, a kind of method that reclaims pure triglycol behind the purified natural gas that contains impurity such as oil, water, ethylene glycol the discarded triglycol solution is applicable to that the regeneration of waste tri-glycol solution is recycled.
Background technology
Triglycol is widely used in each big gas field as the dewatering agent of excellent property in the natural gas conditioning process, but because of the complicacy of Natural gas extraction, all has the contaminated situation of triglycol.Long celebrating gas field gas dehydration, pollutes triglycol and not only influences the decontamination effect improving of Sweet natural gas, even cause the obstruction of natural gas conditioning equipment nearly 15 tons of contaminated depleted in 1999 with triglycol, has a strong impact on the normal exploitation of Sweet natural gas.
Contaminated triglycol is in the past as waste disposal, severe contamination environmental quality, cause very big financial loss simultaneously, triglycol dehydration be after the Sweet natural gas extraction must through one of surface technology process, and be preliminary treatment is carried out at long celebrating all individual well stations, gas field to Sweet natural gas primary process.Therefore, the amount of withdrawing from when batch consumption of annual solution and maintenance is very big, and to the end of the year 2000, the waste tri-glycol that the annual maintenance of 48 cover dehydration sleds of long celebrating gas field is changed reaches 84 tons.Simultaneously, because the complicacy that the special conditions of Sweet natural gas high pressure exploitation and natural gas conditioning are handled, be easy to cause the pollution, rotten of triglycol, make the makings of Sweet natural gas can't be up to standard.
Technology contents
The object of the present invention is to provide the recycling of waste tri-glycol, not only can save very large cost, the difficult problem when having solved triglycol simultaneously and the problem of environmental pollution that may cause as waste disposal.
The present invention is achieved in that
Utilize the bigger boiling-point difference distance of triglycol and other impurity, adopt the method for disposable underpressure distillation to reclaim triglycol, its concrete steps are pressed following process flow diagram:
Total system pressure is lower than-0.08Mpa, the controllable temperature heating system, when distillation temperature is 20 ~ 180 ℃, distill out first fraction of light materials such as condensate oil, water, ethylene glycol, when temperature reaches 180 ~ 190 ℃, distill out second fraction of faint yellow, transparent triglycol product, when temperature rises to more than 200 ℃, residue blackout, the 3rd fraction that viscosity is bigger are residue on evaporation.The present invention also adopts following technical scheme:
Adopt direct disposable distillation under vacuum can satisfy the triglycol product requirement.
The underpressure distillation operational condition is determined at the boiling point under the vacuum tightness according to triglycol main body product.
Second fraction of overhead product is promptly collected as the triglycol product, and bottoms comprises degraded product for the high boiling substance of the macromolecule of no water-retaining capacity.
The heating system of controllable temperature is characterized in that adopting the Sweet natural gas heating system.
The oil bath of the technical process of being adopted, its special sex character are the thermal conductance oil that adopts more than 300 ℃.
Drainer in the technical process of being adopted, the method for cooling of the cool concealed of employing water is quickly cooled to below 40 ℃ the gas phase that steams.
According to the contaminated analysis of causes of triglycol, the essential substance that causes triglycol to pollute is condensation oils, salt, partially decomposed product and other solid impurity.Condensation oils, degradation production and part light materials, its boiling point is lower than triglycol, and salt and other solid impurity boiling point all are higher than triglycol.Therefore, can adopt the distillatory method that each component is separated according to the boiling point difference of polluting each composition of triglycol solution;
Can find from the physico-chemical parameter of triglycol, the boiling point of triglycol is than its theoretical decomposition temperature height, if adopt the method for straight run distillation to purify waste tri-glycol liquid, triglycol was decomposed before boiling point,, reduce the boiling point of triglycol as adopting the method for underpressure distillation, when being lower than the triglycol decomposition temperature, its evaporation is distillated, waste tri-glycol all can be purified recovery, can prevent the decomposition of triglycol again, help recycling waste tri-glycol.
The principle of institute of the present invention foundation is organic underpressure distillation principle, and promptly the boiling point of liquid reduces with the rising of vacuum tightness, its boiling point difference of different liqs.The separation of in view of the above labile triglycol under high boiling point and the high temperature being vaporized under lower temperature.
Description of drawings
Accompanying drawing is that waste tri-glycol reclaims process flow sheet.
Concrete enforcement
Shown in the technological process block diagram, its operational condition:
Require total system pressure to be lower than-0.08Mpa, the controllable temperature heating system, when distillation temperature is 20～180 ℃, distill out first fraction of light materials such as condensate oil, water, ethylene glycol, when temperature reaches 180～190 ℃, distill out second fraction of faint yellow, transparent triglycol product, it does not contain benzene, aromatic hydrocarbons, olefines material, when temperature rose to more than 200 ℃, residue blackout, the 3rd fraction that viscosity is bigger were residue on evaporation.
Heating system adopts the heating system of Sweet natural gas and other controlled humidity:
The thermal conductance oil more than 300 ℃ is adopted in oil bath;
The retort heat exchange is even, and heat interchanging area satisfies distillation institute heat requirement;
Drainer adopts water-cooled or other type of cooling, and 200 ℃ gases are quickly cooled to below 40 ℃;
Waste product storage tank, product storage tank satisfy pressure and disposable distillatory solution reserves;
Surge tank satisfies pressure, and guarantees system pressure smooth change when operation;
Vacuum pump can satisfy the vacuum tightness requirement, and normal load is less than-0.08Mpa.
According to the principle of underpressure distillation, special test apparatus is connected according to design cycle, under the certain vacuum pressure condition that vacuum pump forms, sample is heated, and the fraction and the volume of record differing temps different time sections.
| The sample title | Amount of samples mL | Vacuum pressure mmHg | Distillation temperature ℃ | Cut point ℃ | Produce fraction amount mL | The fraction title |
| Waste tri-glycol | ????100 | 360 | ?20～180 | ?60～180 | ?10 | First fraction |
| 360 | ?185～ | ?190～ | ?80 | Second fraction | ||
| 360 | ?＞200 | ?＞200 | ?10 | The 3rd fraction | ||
| Remarks | The complete blackening of the 3rd fraction, viscosity is bigger, stops distillation | |||||
Analyze the composition of each fraction of underpressure distillation gained, simultaneously with newly go into the qualified triglycol comparative analysis of factory, by the result as can be known second fraction be required product.Assay such as following table:
| Title | Project | Second fraction | Fresh triglycol |
| The quality test index | Outward appearance | Faint yellow, transparent | Little yellow, transparent |
| Colourity | ??3 | ??2 | |
| Moisture | ??0.9293 | ??0.4229 | |
| Density g/cm3 | ??1.1250 | ??1.1248 | |
| The physical and chemical performance index | PH value | ??6.00 | ??6.66 |
| Refractive index | ??1.4574 | ??1.4572 | |
| Form | ??HEG，H 2O，DEG | ??HEG，H 2O，DEG | |
| Suspended substance | ??0 | ??0 | |
| Total glycol content | ??98.08 | ??99.58 |
The invention effect
The qualified triglycol that will reclaim in 2000 connects nearly month of input utilization at northern 2 stations dehydration sled, and its result of use is monitored, and record of production is as follows:
| The well station | Analyze the date | Handle tolerance | The reboiler temperature | The triglycol internal circulating load | Water dew point ℃/4.5Mpa | Rich solution concentration % | Lean solution concentration % |
| North 2 | ?11.1 | 460,000 | 189 | ?313L | -8 | ||
| North 2 | ?11.1 | 460,000 | 192 | ?375L | -9 | ||
| North 2 | ?11.2 | 430,000 | 190 | ?313L | -9 | ?96.9 | ?98.0 |
| North 2 | ?11.2 | 430,000 | 190 | ?313L | -9 |
North 2 platform tickets dehydration sled is the treatment capacity in 500,000 side/skies, under the fully loaded working conditions, satisfies the requirement that natural gas conditioning is produced.
Calendar year 2001 is limited owing to withdrawing from the scrap rate solution amount, device migration in addition, and nearly one month of device operation, 9 tons of output triglycol amounts all are used for production.A part is used for station, south-11, and a part is used for operation one district gas gathering station, any unusual production phenomenon do not occur.
At the bottom of calendar year 2001, the existing gas gathering station in long celebrating gas field builds dehydration sled totally 48 covers, and adding up to the gas conditioning ability is 50 * 10
8m
3/ a, from gas field development longterm planning, this treatment capacity can satisfy to 2003.Once calculate according to the annual maintenance of 48 cover dehydration sleds, each waste tri-glycol of changing reaches 84 tons.According to test-results, the rate of recovery of waste tri-glycol is pressed 60% Schwellenwert budget, and regenerating unit is by the day output that goes back to receive the pure triglycol of 400kg every day, 50 * 10
8m
3In the production capacity period of/a, the annual operation of a covering device can be reclaimed waste tri-glycol in 130 days.By 2005, the gas field is produced and built was 100 * 10
8m
3During/a, regenerating unit also can satisfy the recovery requirement; To 2010, the gas field is produced and built was 200 o'clock, increased by a cover regenerating unit.
(1), when waste tri-glycol does not reclaim, the annual expense prediction in gas field with triglycol
The triglycol amount that the annual maintenance of existing 48 cover dehydration sleds of long celebrating gas field is once changed needs 84 tons, consider the triglycol loss in the production process, need to replenish 150 tons of new triglycols every year, 10000 yuan of triglycol market value per ton, the long celebrating gas field annual master plan of triglycol that needs of existing gas gathering station 48 cover dehydration sleds is paid wages 2,340,000 yuan.
(2), after the waste tri-glycol regenerating unit operation, the annual expense prediction in gas field with triglycol
1, cost of equipment:
Equipment cost, process cost: 120000 element device mounting costs: 30000 yuan of totals: 150000 yuan
2, equipment year depreciation funds: 150000 ÷ 5=30000 units
3, device operation day is expended usefulness:
Day energy charge: 8KW * 24h * 0.75 yuan=144.00 yuan
Daily natural gas expense: 50m
3* 24h * 0.60 yuan=720.00 yuan
From expenses of labour: 2 people * 20 yuan=40 yuan of totals: 904 yuan
3, in the gas field 50 * 10
8m
3During/a production capacity, annual expense of saving the triglycol input: 84 tons * 60% * 10000 yuan-904 yuan * 130-30000=356480 unit.
(3), the gas field different produce build period triglycol regenerating unit economic benefit forecast according to the gas field with the go back working cost of receiving apparatus of the consumption of triglycol and waste tri-glycol, now difference produced the expense joint situation of propping up in the period of building be listed as follows:
(the saving rate is 60% Schwellenwert calculating with the rate of recovery in the table).From table data as can be seen, the putting into operation of waste tri-glycol regenerating unit, the saving rate of annual input expense for the gas field triglycol does not have greater than more than 15%.Therefore, applying of waste tri-glycol regenerating unit will obtain considerable economic benefit.7. schema and brief description waste tri-glycol reclaim technical process such as figure below: under negative pressure, material flows into retort automatically by feed-pipe, closes the charging valve after reaching the scale of the distillation solvent volume that requires; Guarantee vacuum pressure be lower than-the 0.08Mpa condition under, slowly heat oil bath, according to the boiling point control Heating temperature of different fractions; The different fractions gas becomes liquid through condenser, according to the boiling point of each component, product and waste product is diverted to storage tank respectively.When volume of material reaches minimum requirements in to be distilled jar, stop heating, the cooling back replenishes material; The canned bucket of product back sampling analysis.
| The product amount of building (10 8m 3/a) | 50 | ?100 | ?200 |
| Triglycol expenses when not reclaiming (ten thousand yuan) | 234 | ?468 | ?936 |
| Triglycol expenses during recovery (ten thousand yuan) | 198.4 | ?390.7 | ?791.5 |
| Reduce expenses | 35.6 | ?74.3 | ?144.5 |
| Saving rate (%) | 15.2 | ?15.9 | ?15.4 |
Claims (7)
1, the recycling of waste tri-glycol is characterized in that: it is to utilize triglycol and the bigger boiling-point difference distance of other impurity, adopts the method for disposable underpressure distillation to reclaim triglycol, and its concrete steps are pressed following process flow diagram:
Total system pressure is lower than-0.08Mpa, the controllable temperature heating system, when distillation temperature is 20～180 ℃, distill out first fraction of light materials such as condensate oil, water, ethylene glycol, when temperature reaches 180～190 ℃, distill out second fraction of faint yellow, transparent triglycol product, when temperature rises to more than 200 ℃, residue blackout, the 3rd fraction that viscosity is bigger are residue on evaporation.
2. according to the recycling of claims 1 described waste tri-glycol, it is characterized in that: adopt direct disposable distillation under vacuum.
3. press the recycling of letter of authorization 1 described waste tri-glycol, it is characterized in that: the underpressure distillation operational condition is determined at the boiling point under the vacuum tightness according to triglycol main body product.
4. according to the recycling of claims 1 described waste tri-glycol, it is characterized in that: second fraction of overhead product is promptly collected as the triglycol product, and bottoms comprises degraded product for the high boiling substance of the macromolecule of no water-retaining capacity.
5. press the recycling of claims 1 described waste tri-glycol, it is characterized in that: the heating system of controllable temperature is to adopt the Sweet natural gas heating system.
6. press the recycling of claims 1 described waste tri-glycol, it is characterized in that: the oil bath of the technical process of being adopted in the recovery method, adopt the thermal conductance oil more than 300 ℃.
7. press the recycling of claims 1 described waste tri-glycol, it is characterized in that: the drainer in the technical process is the method for cooling that adopts the cool concealed of water, and the gas phase that steams is quickly cooled to below 40 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021237794A CN1465559A (en) | 2002-06-28 | 2002-06-28 | Recycling of waste triethylene glycol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021237794A CN1465559A (en) | 2002-06-28 | 2002-06-28 | Recycling of waste triethylene glycol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1465559A true CN1465559A (en) | 2004-01-07 |
Family
ID=34142475
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA021237794A Pending CN1465559A (en) | 2002-06-28 | 2002-06-28 | Recycling of waste triethylene glycol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1465559A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101773749A (en) * | 2010-03-01 | 2010-07-14 | 新疆石油学院 | Method for purifying polyol for preventing natural gas from freezing and dehydrating natural gas and equipment |
| CN101007758B (en) * | 2006-11-09 | 2011-04-27 | 上海金海雅宝精细化工有限公司 | Crystallized mother liquor recovery process during anti-oxidant production process |
| CN106518633A (en) * | 2016-10-17 | 2017-03-22 | 中石化上海工程有限公司 | Method for producing high-purity triethylene glycol |
| CN106542975A (en) * | 2016-10-17 | 2017-03-29 | 中石化上海工程有限公司 | The method of continuous production high-purity triethylene glycol |
| CN113737293A (en) * | 2021-06-30 | 2021-12-03 | 桐昆集团股份有限公司 | Filter element triethylene glycol washs and recycle device |
-
2002
- 2002-06-28 CN CNA021237794A patent/CN1465559A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101007758B (en) * | 2006-11-09 | 2011-04-27 | 上海金海雅宝精细化工有限公司 | Crystallized mother liquor recovery process during anti-oxidant production process |
| CN101773749A (en) * | 2010-03-01 | 2010-07-14 | 新疆石油学院 | Method for purifying polyol for preventing natural gas from freezing and dehydrating natural gas and equipment |
| CN101773749B (en) * | 2010-03-01 | 2012-08-22 | 新疆石油学院 | Method for purifying polyol for preventing natural gas from freezing and dehydrating natural gas and equipment |
| CN106518633A (en) * | 2016-10-17 | 2017-03-22 | 中石化上海工程有限公司 | Method for producing high-purity triethylene glycol |
| CN106542975A (en) * | 2016-10-17 | 2017-03-29 | 中石化上海工程有限公司 | The method of continuous production high-purity triethylene glycol |
| CN106518633B (en) * | 2016-10-17 | 2019-04-09 | 中石化上海工程有限公司 | The production method of high-purity triethylene glycol |
| CN106542975B (en) * | 2016-10-17 | 2019-06-11 | 中石化上海工程有限公司 | The method of continuous production high-purity triethylene glycol |
| CN113737293A (en) * | 2021-06-30 | 2021-12-03 | 桐昆集团股份有限公司 | Filter element triethylene glycol washs and recycle device |
| CN113737293B (en) * | 2021-06-30 | 2022-08-30 | 桐昆集团股份有限公司 | Filter element triethylene glycol washs and recycle device |
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