CN1037505C - Treating method for discharged alkali liqnid of synthesizing octene aldehyde system - Google Patents
Treating method for discharged alkali liqnid of synthesizing octene aldehyde system Download PDFInfo
- Publication number
- CN1037505C CN1037505C CN92103260A CN92103260A CN1037505C CN 1037505 C CN1037505 C CN 1037505C CN 92103260 A CN92103260 A CN 92103260A CN 92103260 A CN92103260 A CN 92103260A CN 1037505 C CN1037505 C CN 1037505C
- Authority
- CN
- China
- Prior art keywords
- alkali lye
- process according
- treatment process
- falling
- film evaporator
- 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.)
- Expired - Fee Related
Links
- 239000003513 alkali Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims description 27
- -1 octene aldehyde Chemical class 0.000 title claims description 8
- 230000002194 synthesizing effect Effects 0.000 title claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011552 falling film Substances 0.000 claims abstract description 23
- 239000010865 sewage Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 14
- 238000004587 chromatography analysis Methods 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000013375 chromatographic separation Methods 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 66
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 16
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 4
- 150000001299 aldehydes Chemical class 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000005273 aeration Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
Landscapes
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
In the octenal synthesis reaction, due to the generation of water, alkali liquor which is used as a catalyst is diluted. The diluted alkali liquor discharged out of an octenal reaction system is treated by the present invention, and the diluted alkali liquor has the alkalinity of 0.8 to 1.3% (weight) and has the CODcr concentration of 30000 to 50000 mg/1. The diluted alkali liquor is treated by a depressurization falling-film evaporation-stripping technology, the evaporated concentrated alkali liquor can be sent back to the reaction system to be continuously used, and part of the evaporated water is treated by the stripping technology. The CODcr concentration of water can be reduced below 1000 mg/1 after the stripping, and the water can be discharged to a common sewage treatment device.
Description
The present invention relates to a kind of treatment process of organic reaction system discharging alkali lye, relate in particular to a kind of treatment process of synthesizing octene aldehyde reactive system discharging alkali lye.
Octenal is an intermediate of producing octanol with butyraldehyde, contracts at butyraldehyde two and produces in the reactive system of octenal, and alkali (NaOH) liquid that adopts 2% (weight) is as catalyzer.When butyraldehyde two contracts generation a part octenal, be accompanied by and generate a part water, so just diluted alkaline solution as catalyzer, in order to keep the concentration of alkaline catalysts, must from system, discharge a part of sig water continuously, mend a part of high alkali liquid simultaneously, the sig water of discharging as sewage is exactly the present invention's alkali lye to be processed.This strand sig water is less owing to discharge capacity, alkalinity height (0.7-1.3% (weight)), and CODcr concentration contains the raw material butyraldehyde simultaneously and reaches isobutyric aldehyde and the product octenal of bringing into raw material, by product butanols, isopropylcarbinol etc. up to 30000-50000mg/L.If entering common sewage treatment facility (as biological treatment device), this strand alkali lye can impact the normal running of sewage treatment facility; Simultaneously, because the continuous discharge of sig water, the consumption of alkali is very big in the reactive system, and process cost increases.
Processing to this kind water, do not see relevant report both at home and abroad as yet, adopt evaporation-burning-causticization for the recovery of alkali lye more, obtain NaOH at last, energy consumption is big on the one hand for the method that is proposed as Chinese patent CN88105855A, it only pays attention to the recovery of alkali on the other hand, does not consider the processing to pollutent.Japanese Patent clear 5330479 has been introduced the treatment unit that contains the volatile organic matter waste liquid, it is with the whole or most of evaporations of waste liquid substantially, enter the vapor phase catalytic oxidation reactor then, vapor phase catalytic oxidation reactor service temperature requires 300 ℃, high-temperature steam is made thermal source, and the catalyzer that requires multiple metal composite is (as Pt-Al
2O
3), pressurized air is made oxygen source, and therefore investment and process cost are all very high, and this patent does not illustrate final treatment effect.
The purpose of this invention is to provide a kind of new method, alkali is back to use in the system goes, and make water after the processing can enter common sewage treatment facility and do not impact.
Because when temperature is higher, condensation reaction can take place in octenal, adopt the decompression falling film evaporation can reduce vaporization temperature, simultaneously can steam some volatile organic matters as much as possible, the component of maintenance system can not increase again, alkali lye after concentrating can be squeezed into reactor and continue to use, and the hydromining that steams is further handled with stripping process, and the water after stripping is handled can enter common sewage treatment facility and not impact.
Accompanying drawing 1 has been described technical process of the present invention, wherein
(1)-the alkali lye surge tank;
(2)-the decompression falling-film evaporator;
(3)-vapour liquid separator;
(4)-surge tank;
(5)-the chromatography device;
(6)-stripping tower;
(7)-surge tank;
(8)-give hot device;
(9) (10)-condenser;
A-alkali lye feeding line;
B-falling-film evaporator heating steam line;
C-vapour liquid separator feeding line;
D-concentrate alkali lye to discharge line;
E-chromatography device organism and oil are discharged line;
F-stripping tower feeding line;
Line is discharged in h-stripping water outlet;
G-stripping tower stripped vapor line.
Accompanying drawings specific implementation process of the present invention:
The alkali lye of synthesizing octene aldehyde system discharging is entered alkali lye surge tank (1), slow by alkali lye Rushing tank (1) gives after hot device (8) and enters decompression falling film evaporator (2) falling liquid film that reduces pressure after the heat and steam Send out, the liquid-vapor mixture of the alkali lye after the evaporation enters vapour liquid separator (3) and carries out vapor-liquid separation, Liquid phase part-namely concentrate alkali lye return the synthesizing octene aldehyde reaction system via the d line and continue The continuous use, the vapour phase part enters surge tank (4) after condenser (9) condensation, by surge tank (4) Squeeze into chromatography device (5), the organic matter on chromatography device (5) upper strata and oil discharge to reclaim via the e line or Burn, the draining of chromatography device (5) lower floor is squeezed into the top of stripper (6) via surge tank (7), Stripping is walked the g line with steam, and the stripping water outlet of stripper (6) bottom can enter common dirt Water processing establishment, the vapour phase part at stripper (6) top enters layer after condenser (10) condensation Parser (5) carries out chromatography.
In said process, vacuum pump is connected with condenser (9), the vacuum tightness of control falling-film evaporator (2), vapour liquid separator (3) and condenser (9).Because the octenal in the alkali lye contacts very easily oxidation with butyraldehyde, for preventing the air admission vacuum system, alkali lye surge tank (1) adopts airtight air form and keeps malleation with rare gas element, in the present invention, adopt nitrogen to keep the pressure of alkali lye surge tank (1), the pressure of alkali lye surge tank (1) will be to guarantee that alkali lye can enter falling-film evaporator (2) smoothly and be as the criterion.The concentration ratio of temperature, pressure and alkali lye that falling-film evaporator (2) inner control is certain, the working pressure in the falling-film evaporator in Ben Biming (2) is 2.66 * 10
4Pa～4.0 * 10
4Pa, corresponding service temperature (i.e. the boiling point of Dui Ying solution) is 66-75 ℃; The temperature out of the temperature of falling-film evaporator charging alkali lye-promptly give hot device (8) alkali lye preferably adopts the bubble point temperature of the alkali lye under falling-film evaporator (2) working pressure, because of the bubble point temperature charging can improve evaporative process; The concentration ratio of the alkali lye in the falling-film evaporator (2) is controlled at 30-70%, preferably is controlled at 40-60%.Vapour liquid separator is provided with defoaming device in (3), and the defoaming device of Cai Yonging is a metallic sieve in the present invention.The working pressure of stripping tower (6) is 1.7 * 10
5Pa～2.5 * 10
5Pa, service temperature is 118 ℃ ± 10 ℃ at the bottom of the tower of stripping tower (6), the steam rate of stripping tower (6) water is controlled at 4-20% (weight), preferably is controlled at 6-10% (weight).
Hereto, the present invention has finished the processing of discharged alkali liqnid of synthesizing octene aldehyde system, has realized the reuse of alkali lye and the purpose that the waste water after the processing can enter common sewage treatment facility.
The alkali lye of synthesizing octene aldehyde system discharging is handled through method of the present invention, and can make concentration is that the sig water of 0.8-1.3% (weight) is concentrated into 1.6-2.6% (weight), and does not increase new organic component, reaches reusable purpose.The CODcr concentration of water can be controlled at below the 1000mg/L behind the stripping, and the content of material such as the butanols in the water, octenal seldom, can not impact to common sewage treatment facility (as biochemical aeration tank etc.).The organism and the oil of discharging in the chromatography device (5) can reclaim or burn.
The method that the method for alkali and evaporation-vapour phase wet oxidation are reclaimed in the present invention and evaporation has fully been compared and has been saved energy, alkali lye reuse and waste water and advantage such as effectively administered.
Embodiment
Example 1 example 2 sig water character CODcr, mg/l 45,935 37524 basicity % (weight) 1.27 0.81 isobutyric aldehydes, mg/l does not detect＜10 butyraldehyde, mg/l 109 129 isopropylcarbinols, mg/l 52 214 butanols, mg/l 248 1876 octenals, mg/l 1,878 1576 enters falling-film evaporator (2) alkali lye amount, the steam consumption of T/hr 15.3 13.6 falling-film evaporators (2), T/hr 16.8 14.9 vapor pressures, Pa 2.5 * 10
52.5 * 10
5Vapor temperature, the service temperature of ℃ 127 127 falling-film evaporators (2), the working pressure of ℃ 66 68 falling-film evaporators (2), Pa 2.66 * 10
43.0 * 10
4The pressure of alkali lye surge tank (1), Pa 3.0 * 10
53.0 * 10
5The operating pressure of vapour liquid separator (3), Pa 2.56 * 10
42.90 * 10
4Concentrate character basicity % (weight) 2.33 1.67 isobutyric aldehydes of alkali lye, mg/l does not detect butyraldehyde, mg/l 52 40 isopropylcarbinols, mg/l does not detect 35 butanols, mg/l 26 236 octenals, mg/l 274 44 concentrates the alkali lye amount, T/hr 8.3 6.6 stripping tower flooding quantitys, T/hr 7.0 7.0 stripping tower quantity of steams, T/hr 1.63 1.63 stripping tower column bottom temperatures, ℃ 118 118 stripping tower working pressures, Pa 1.7 * 10
51.7 * 10
5The character CODcr of water outlet behind the stripping, mg/l 900 800 isobutyric aldehydes, mg/l does not detect butyraldehyde, mg/l does not detect isopropylcarbinol, mg/l does not detect butanols, mg/l 16 26 octenals, mg/l＜10 147 water stripping steam rate % (weight) 9.6 6.0
Claims (11)
1, a kind of method that is used to handle discharged alkali liqnid of synthesizing octene aldehyde system, wherein, the alkali lye of system discharging is entered falling-film evaporator (2) falling film evaporation of reducing pressure by surge tank (1) through giving hot device (8), it is characterized in that, alkali lye after the evaporation is after vapour liquid separator (3) separates, the alkali lye that liquid phase part has concentrated is returned reactive system and is continued to use, the vapour phase part enters chromatography device (5) chromatographic separation after condenser (9) condensation, organism or the recovery that discharge on chromatography device (5) upper strata or burn, the draining of chromatography device (5) bottom is squeezed into the top of stripping tower (6) and is carried out the stripping processing, the stripping water outlet of stripping tower (6) bottom enters common sewage treatment facility, and the vapour phase part at stripping tower (6) top enters chromatography device (5) and carries out chromatographic separation after condenser (10) condensation.
2, treatment process according to claim 1 is characterized in that alkali lye surge tank (1) is airtight and keep alkali lye surge tank malleation with rare gas element, so that alkali lye can successfully enter falling-film evaporator (2).
3, treatment process according to claim 2 is characterized in that lazy feelings gas adopts nitrogen.
4, treatment process according to claim 1, the working pressure that it is characterized in that falling-film evaporator (2) is 2.66 * 10
4Pa-4.0 * 10
4Pa, service temperature is 66-75 ℃.
5, treatment process according to claim 4, the alkali lye feeding temperature that it is characterized in that falling-film evaporator (2) is controlled at the alkali lye bubble point temperature under the working pressure.
6, treatment process according to claim 1 is characterized in that in the vapour liquid separator (3) defoaming device being housed, and adopts metallic sieve.
7, treatment process according to claim 1, the working pressure that it is characterized in that stripping tower (6) is 1.7 * 10
5Pa～2.5 * 10
5Pa, service temperature is 118 ℃ ± 10 ℃ at the bottom of the tower.
8, treatment process according to claim 1 is characterized in that the concentration ratio of the interior alkali lye of falling-film evaporator (2) is controlled at 30-70%.
9, treatment process according to claim 8 is characterized in that the concentration ratio of the interior alkali lye of falling-film evaporator (2) is controlled at 40-60%.
10, treatment process according to claim 1 is characterized in that the steam rate of the interior water of stripping tower (6) is controlled at 4-20%.
11, treatment process according to claim 10 is characterized in that the interior evaporation of water of stripping tower (6) goes out rate and is controlled at 6-10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92103260A CN1037505C (en) | 1992-05-07 | 1992-05-07 | Treating method for discharged alkali liqnid of synthesizing octene aldehyde system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92103260A CN1037505C (en) | 1992-05-07 | 1992-05-07 | Treating method for discharged alkali liqnid of synthesizing octene aldehyde system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1065642A CN1065642A (en) | 1992-10-28 |
| CN1037505C true CN1037505C (en) | 1998-02-25 |
Family
ID=4940101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92103260A Expired - Fee Related CN1037505C (en) | 1992-05-07 | 1992-05-07 | Treating method for discharged alkali liqnid of synthesizing octene aldehyde system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1037505C (en) |
-
1992
- 1992-05-07 CN CN92103260A patent/CN1037505C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1065642A (en) | 1992-10-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3875019A (en) | Recovery of ethylene glycol by plural stage distillation using vapor compression as an energy source | |
| CN104926653A (en) | Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device | |
| US4758650A (en) | Process and apparatus for producing high molecular weight polyesters | |
| CN104926655A (en) | Technology and device for diethyl oxalate synthesis through vapor permeation dehydration process | |
| CN111643915A (en) | Rectification device and rectification method for oxo-synthesis of acetic acid | |
| CN217163255U (en) | A rectification equipment that is arranged in N-methylaniline production methyl alcohol to retrieve | |
| CN1280102A (en) | Treatment and source recovering method for waste water of 1,4-dihydroxy anthraquinone produetion | |
| CN1037505C (en) | Treating method for discharged alkali liqnid of synthesizing octene aldehyde system | |
| CN209098188U (en) | A kind of hydrogen peroxide concentration purifying plant | |
| CN1306450A (en) | Process for treatment of waste water | |
| CN108424350A (en) | A kind of technique of purification medicinal ethyl alcohol | |
| CN112552146B (en) | Purification method of by-product ethylene glycol from polyester conversion to plasticizer | |
| US4675420A (en) | Generation of reduced pressure in apparatuses in the preparation of phthalic anhydride and maleic anhydride | |
| KR20230010260A (en) | Separation method and reactor system for glycol-water mixtures | |
| CN111821821A (en) | Device and method for recycling fusel oil in methanol production | |
| CN219972045U (en) | Aldehyde-containing wastewater treatment process device for methyl acrylate and methyl methacrylate production process | |
| CN114432728B (en) | System and process for purifying NMP | |
| CN1333204A (en) | Method and device for hydrolyzing methyl acetate | |
| CN216549990U (en) | Waste liquid recycling system | |
| CN212594874U (en) | Fusel oil cyclic utilization device in methanol production | |
| CN109467499B (en) | Anticorrosion process and device for hydrolysis of methyl acetate and purification of acetic acid in the process of recovery of polyvinyl alcohol mother liquor | |
| CN219023294U (en) | Methacrylic acid purifying device | |
| CN109550359B (en) | Utilization method for recovering components in purge gas by using efficient absorbent | |
| SU1404099A1 (en) | Method of regeneration of saturated solution of glycol | |
| CN220642657U (en) | Sewage treatment system of high-pressure evaporation reflux tank |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: CHINA PETROLEUM & CHEMICAL CORPORATION, FUSHUN PET Free format text: FORMER NAME OR ADDRESS: FUSHUN PETROCHEMICAL INSTITUTE., CHINA PETROCHEMICAL CORP. |
|
| CP01 | Change in the name or title of a patent holder |
Patentee after: Sinopec Group Fushun Research Institute of Petroleum and Petrochemicals Patentee before: Fushun Research Inst. of Petroleum Processing, China Petro-chem. Corp. |
|
| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
| OR01 | Other related matters | ||
| ASS | Succession or assignment of patent right |
Owner name: CHINA PETROLEUM AND CHEMICAL CORPORATION FUSHUN P Free format text: FORMER OWNER: CHINA PETROLEUM + CHEMICAL CORPORATION, FUSHUN PETROL-CHEMICAL INSTITUTE Effective date: 20071019 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20071019 Address after: The eastern section of Dandong road 113001 in Liaoning province Fushun City Wanghua District No. 31 Patentee after: Sinopec Fushun Research Institute of Petroleum and Petrochemicals Address before: Dandong road Wanghua District 113001 Liaoning city of Fushun Province Patentee before: Sinopec Group Fushun Research Institute of Petroleum and Petrochemicals |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 19980225 Termination date: 20100507 |