CN115785034A - System for recovering furfural from phenolic resin waste liquid and recovery method thereof - Google Patents
System for recovering furfural from phenolic resin waste liquid and recovery method thereof Download PDFInfo
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- CN115785034A CN115785034A CN202211584073.0A CN202211584073A CN115785034A CN 115785034 A CN115785034 A CN 115785034A CN 202211584073 A CN202211584073 A CN 202211584073A CN 115785034 A CN115785034 A CN 115785034A
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- furfural
- rectifying tower
- waste liquid
- tower
- phenolic resin
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 166
- 239000007788 liquid Substances 0.000 title claims abstract description 32
- 239000002699 waste material Substances 0.000 title claims abstract description 29
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 22
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000011084 recovery Methods 0.000 title claims abstract description 11
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 20
- 238000010992 reflux Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000006482 condensation reaction Methods 0.000 abstract description 8
- 238000009833 condensation Methods 0.000 abstract description 6
- 230000005494 condensation Effects 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 208000005156 Dehydration Diseases 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical group C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N ortho-diethylbenzene Natural products CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The application relates to the field of organic solvent recovery, in particular to a system for recovering furfural from phenolic resin waste liquid and a recovery method thereof. A system for recovering furfural from a phenolic resin waste liquid comprises: the heavy component is provided with a first rectifying tower, and the first rectifying tower is used for carrying out heavy component removal treatment on the phenolic resin waste liquid so as to remove phenol; the purification assembly is arranged on one side of the de-weight assembly and communicated with the de-weight assembly, and a second rectifying tower is arranged in the purification assembly to purify the de-weight processed components in the first rectifying tower. The method comprises the following steps: s1, removing weight and layering; and S2, azeotropic distillation. According to the method, phenol which is easy to generate condensation reaction is separated and then refined by furfural through double-tower combined transportation. Reduce solid residue produced by condensation and improve the rectification yield. Meanwhile, oxygen in the furfural is removed through negative pressure rectification of the furfural, the color of the furfural is improved, and the purity of the furfural is further improved.
Description
Technical Field
The application relates to the field of organic solvent recovery, in particular to a system for recovering furfural from phenolic resin waste liquid and a recovery method thereof.
Background
Furfural, also known as furaldehyde, is a colorless, transparent liquid with an almond-flavored odor, is dissolved in hot water, ethanol, diethyl ether and benzene, and is gradually oxidized in the air to become yellow to tan. Since it contains a furan ring and an aldehyde group, a large number of derivatives can be prepared by oxidation, hydrogenation, condensation and other reactions. Furfural is an important organic chemical raw material obtained by hydrolyzing biomass, and is a renewable and green chemical product. Can be widely applied to the fields of food, medicine, pesticide, chemical industry and the like, and can be used for synthesizing and preparing biodegradable high polymer materials.
Aiming at the related technologies, the inventor finds that a large amount of furfural exists in the phenolic resin waste liquid, if the furfural is directly incinerated, the waste of resources is caused, a large amount of coking is caused in a tower kettle to form phenolic resin through a high-temperature condensation reaction in the ordinary single-tower rectification, the yield is greatly reduced, and the caking of materials in the whole rectification tower kettle can be caused in severe cases. When phenol and furfural coexist, condensation reaction can occur, water is generated to influence the quality of finished products, and furfural acid coking formed by contact of furfural and oxygen can influence the use of fillers and equipment.
Disclosure of Invention
In order to improve the current poor defect of effect of retrieving furfural in the phenolic resin waste liquid, the application provides a system of retrieving furfural from the phenolic resin waste liquid and recovery method thereof.
In a first aspect, the application provides a system for recovering furfural from phenolic resin waste liquid, which adopts the following technical scheme:
a system for recovering furfural from a phenolic resin waste liquid comprises:
the heavy component is provided with a first rectifying tower, and the first rectifying tower is used for carrying out heavy component removal treatment on the phenolic resin waste liquid so as to remove phenol;
the purification assembly is arranged on one side of the de-weight assembly and communicated with the de-weight assembly, and a second rectifying tower is arranged in the purification assembly to purify the de-weight processed components in the first rectifying tower.
By adopting the technical scheme, the scheme of double-rectifying-tower combined transportation is adopted, and by double treatment of weight removal and purification, phenol which generates condensation reaction is separated and then furfural is refined, so that solid residues generated by condensation are reduced, and the yield and quality of rectification are improved.
Preferably, the first rectifying column includes:
the delayer is arranged at one end of the top of the first rectifying tower and used for collecting and separating furfural and moisture in the rectifying components of the first rectifying tower.
By adopting the technical scheme, the delayer can effectively separate the furfural from the phenol, so that the phenomenon that the phenol is easy to generate condensation reaction in the furfural refining process is effectively improved, and the yield and the quality of rectification are improved.
In a second aspect, the present application provides a method for recovering furfural from a phenolic resin waste liquid, comprising the following recovery steps:
s1, removing a heavy layer: taking waste liquid, placing the waste liquid in a weight removal component, removing phenol in a tower kettle through weight removal treatment of a first rectifying tower, layering components on the top of the tower through a layering device arranged at one end of the top of the first rectifying tower, and collecting lower-layer materials;
s2, azeotropic distillation: taking the lower layer of material, introducing the lower layer of material into a second rectifying tower, and extracting a furfural finished product through a furfural negative pressure azeotropic rectification side line of the second rectifying tower, thus obtaining the furfural through recovery.
By adopting the technical scheme, the furfural is refined after phenol which is easy to generate condensation reaction is separated through double-tower combined transportation. The solid residue produced by condensation is reduced, and the rectification yield is improved. Furthermore, the furfural is rectified under negative pressure, so that oxygen in the furfural is removed, the color of the furfural is improved, and the purity of the furfural is further improved.
Preferably, the lower layer material in the step S1 includes furfural and water, and the moisture content in the lower layer material is less than 10%.
Preferably, the pressure of the heavy metal removal treatment of the first rectifying tower in the step S1 is 4.8-5.5 kPa, the tower top temperature is 40-50 ℃, and the reflux ratio is 2.5-3.
Preferably, the operating pressure of the negative pressure azeotropic distillation in the step S2 is 5-9 kPa, the top temperature is controlled at 65-68 ℃, and the reflux ratio of the distillation tower is controlled at 2-3.
By adopting the technical scheme, the method further optimizes the scheme of furfural purification, effectively optimizes the parameters of furfural purification, and improves the purity and quality of finally prepared furfural.
In summary, the present application has the following beneficial effects:
firstly, phenol which is easy to generate condensation reaction is separated and then refined by furfural through double-tower combined transportation, so that solid residues generated by condensation are reduced, and the rectification yield is improved.
Secondly, the application reaches the standard of recycling through heterogeneous azeotropic rectification dehydration of furfural, does not need to carry out dehydration treatment through a molecular sieve or a pervaporation membrane, and simultaneously, because the furfural is rectified under negative pressure in the application, oxygen in the furfural is removed, and the finished furfural is colorless and does not change color within 7 days under the protection of nitrogen.
Drawings
Fig. 1 is a schematic structural diagram of a system for recovering furfural from a phenolic resin waste liquid in example 1 of the present application.
Wherein, 1, a first rectifying tower; 11. a filter; 12. a delayer; 2. a second rectifying tower.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Example 1
S1, removing a heavy layer: filtering furfural waste liquid in a filter, collecting filtrate, placing the filtrate in a first rectifying tower, starting a vacuum pump, heating to 90 ℃, controlling the top temperature to be 40 ℃, controlling the operating pressure to be 4.8kPa, controlling the reflux ratio to be 2.5, extracting an azeotrope of furfural and water from the top of the first rectifying tower, layering components at the top of the first rectifying tower through a layering device arranged at one end of the top of the first rectifying tower, and collecting lower-layer materials;
s2, azeotropic distillation: taking a lower layer material and introducing the lower layer material into a second rectifying tower, starting a vacuum pump to heat the second rectifying tower until the liquid level of a tower kettle of the second rectifying tower rises to two thirds, wherein the temperature of the tower kettle is 80-85 ℃, the top temperature is 65 ℃, the operating pressure is 5kPa, and the reflux ratio is 2; and continuously dehydrating the tower top, performing negative pressure azeotropic distillation on the furfural in a second rectifying tower, and extracting a furfural finished product at the side line temperature of 70 ℃ to obtain the furfural.
Example 2
S1, removing a heavy layer: filtering furfural waste liquid in a filter, collecting filtrate, placing the filtrate in a first rectifying tower, starting a vacuum pump, heating to 92 ℃, keeping the top temperature at 45 ℃, operating pressure at 5.2kPa, reflux ratio at 2.7, collecting an azeotrope of furfural and water at the top of the first rectifying tower, layering components at the top of the first rectifying tower through a layering device arranged at one end of the top of the first rectifying tower, and collecting lower-layer materials;
s2, azeotropic distillation: taking a lower layer material and introducing the lower layer material into a second rectifying tower, starting a vacuum pump to heat the second rectifying tower until the liquid level of the tower kettle of the second rectifying tower rises to two thirds, wherein the temperature of the tower kettle is 80-85 ℃, the top temperature is 66 ℃, the operating pressure is 7kPa, and the reflux ratio is 2.5; and continuously dehydrating the tower top, performing negative pressure azeotropic distillation on the furfural in a second rectifying tower, and extracting a furfural finished product at the side line temperature of 71 ℃ to obtain the furfural.
It should be noted that, in the present application, furfural subjected to layered treatment by the delayer may enter the second rectifying tower for refining, and may also enter the first rectifying tower for reflux treatment.
Example 3
S1, removing a heavy layer: filtering furfural waste liquid in a filter, collecting filtrate, placing the filtrate in a first rectifying tower, starting a vacuum pump, heating to 95 ℃, keeping the top temperature at 50 ℃, operating pressure at 5.5kPa and reflux ratio at 3, collecting an azeotrope of furfural and water at the top of the first rectifying tower, layering components at the top of the first rectifying tower through a layering device arranged at one end of the top of the first rectifying tower, and collecting lower-layer materials;
s2, azeotropic distillation: taking a lower layer of material and introducing the lower layer of material into a second rectifying tower, starting a vacuum pump to heat the tower kettle to 85 ℃ when the liquid level of the tower kettle of the second rectifying tower rises to two thirds, wherein the top temperature is 68 ℃, the operating pressure is 9kPa, and the reflux ratio is 3; and continuously dehydrating the tower top, performing negative pressure azeotropic distillation on the furfural in a second distillation tower, and extracting a furfural finished product at the side line temperature of 72 ℃, thus recovering the furfural.
Comparative example
Comparative example 1
Compared with the embodiment 1, the pressure of a first rectifying tower in the comparative example is 10kpa, the kettle temperature of the first rectifying tower is 100 ℃, azeotrope of furfural and water is extracted from the top of the tower in an azeotropic mode, a furfural finished product is collected when the top temperature is 76 ℃, and furfural is collected by single-tower rectification.
Performance test
The purity and moisture of furfural recovered in examples 1 to 3 and comparative example 1 were tested, and the specific test results are shown in table 1 below: TABLE 1 Performance test Table
By combining the data of examples 1 to 3 and comparative example 1, the technical scheme of the application can separate phenol which is easy to generate condensation reaction through double-tower combined transportation and then refine furfural. Reduce solid residue produced by condensation and improve the rectification yield. Furthermore, the furfural is rectified under negative pressure, so that oxygen in the furfural is removed, the color of the furfural is improved, and the purity of the furfural is further improved.
Compared with the comparative example 1, it can be further illustrated that the moisture content in the furfural obtained by separating phenol in the embodiments 1 to 3 of the present application is significantly less than the moisture content in the furfural in the comparative example 1.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.
Claims (6)
1. A system for recovering furfural from a phenolic resin waste liquid is characterized by comprising:
the heavy component is provided with a first rectifying tower (1), and the first rectifying tower (1) is used for carrying out heavy treatment on the phenolic resin waste liquid to remove phenol;
the purification assembly is arranged on one side of the heavy component removal assembly and communicated with the heavy component removal assembly, and a second rectifying tower (2) is arranged in the purification assembly to purify the components subjected to heavy component removal in the first rectifying tower (1).
2. A system for recovering furfural from phenolic resin waste liquid according to claim 1, characterized in that the first rectification column (1) comprises:
the delayer (12), the delayer (12) is located the top of the tower one end of first rectifying column (1) is in order to collect and separate furfural and moisture in the first rectifying column (1) rectification component.
3. The method for recovering furfural from a phenol resin waste liquid according to any one of claims 1 to 2, characterized by comprising the following recovery steps:
s1, removing a heavy layer: taking waste liquid, placing the waste liquid in a weight removal component, removing phenol in a tower kettle through weight removal treatment of a first rectifying tower, layering components on the top of the tower through a layering device arranged at one end of the top of the first rectifying tower, and collecting lower-layer materials;
s2, azeotropic distillation: taking the lower layer of material, introducing the lower layer of material into a second rectifying tower, and extracting a furfural finished product through a furfural negative pressure azeotropic rectification side line of the second rectifying tower, thus obtaining the furfural through recovery.
4. The method for recovering furfural from phenol resin waste liquid according to claim 3, characterized in that the lower layer material in step S1 comprises furfural and water, and the moisture content in the lower layer material is less than 10%.
5. The method for recovering the furfural from the phenolic resin waste liquid according to claim 3, wherein the pressure of the de-weighting treatment of the first rectifying tower in the step S1 is 4.8 to 5.5kPa, the tower top is 40 to 50 ℃, and the reflux ratio is 2.5 to 3.
6. The method for recovering the furfural from the phenolic resin waste liquid according to claim 3, wherein the operating pressure of the negative pressure azeotropic distillation in the step S2 is 5 to 9kPa, the top temperature is controlled to be 65 to 68 ℃, and the reflux ratio of the rectifying tower is controlled to be 2 to 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211584073.0A CN115785034A (en) | 2022-12-09 | 2022-12-09 | System for recovering furfural from phenolic resin waste liquid and recovery method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211584073.0A CN115785034A (en) | 2022-12-09 | 2022-12-09 | System for recovering furfural from phenolic resin waste liquid and recovery method thereof |
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| CN202211584073.0A Pending CN115785034A (en) | 2022-12-09 | 2022-12-09 | System for recovering furfural from phenolic resin waste liquid and recovery method thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1537835A (en) * | 1976-05-07 | 1979-01-04 | Bp Chem Int Ltd | Recovery of phenols from aqueous effluents from phenol/aldehyde resin plants |
| CN106588828A (en) * | 2015-10-14 | 2017-04-26 | 中国石化仪征化纤有限责任公司 | Separation and purification method of THF (tetrahydrofuran) distillation waste liquid |
| CN108164482A (en) * | 2016-12-07 | 2018-06-15 | 中糠股份有限公司 | The recovery method and its special equipment of furfural in a kind of aldehyde mud |
| CN109336847A (en) * | 2018-10-23 | 2019-02-15 | 雅邦新材料研发南京有限公司 | A kind of distillation system and its workflow recycling propylene oxide raffinate |
| CN111635381A (en) * | 2020-05-25 | 2020-09-08 | 安徽金禾实业股份有限公司 | Treatment method of furfural rectification waste liquid |
| CN111646960A (en) * | 2020-05-25 | 2020-09-11 | 安徽金禾实业股份有限公司 | Recovery method of furfuryl alcohol in 2-methyl furan wastewater |
| CN113651782A (en) * | 2021-09-02 | 2021-11-16 | 中国矿业大学(北京) | Method for recovering furfural from furfural refining tower bottoms |
| CN115140791A (en) * | 2022-06-06 | 2022-10-04 | 河南汇阳化工科技有限公司 | Device and process for recovering and extracting furfural from process wastewater |
-
2022
- 2022-12-09 CN CN202211584073.0A patent/CN115785034A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1537835A (en) * | 1976-05-07 | 1979-01-04 | Bp Chem Int Ltd | Recovery of phenols from aqueous effluents from phenol/aldehyde resin plants |
| CN106588828A (en) * | 2015-10-14 | 2017-04-26 | 中国石化仪征化纤有限责任公司 | Separation and purification method of THF (tetrahydrofuran) distillation waste liquid |
| CN108164482A (en) * | 2016-12-07 | 2018-06-15 | 中糠股份有限公司 | The recovery method and its special equipment of furfural in a kind of aldehyde mud |
| CN109336847A (en) * | 2018-10-23 | 2019-02-15 | 雅邦新材料研发南京有限公司 | A kind of distillation system and its workflow recycling propylene oxide raffinate |
| CN111635381A (en) * | 2020-05-25 | 2020-09-08 | 安徽金禾实业股份有限公司 | Treatment method of furfural rectification waste liquid |
| CN111646960A (en) * | 2020-05-25 | 2020-09-11 | 安徽金禾实业股份有限公司 | Recovery method of furfuryl alcohol in 2-methyl furan wastewater |
| CN113651782A (en) * | 2021-09-02 | 2021-11-16 | 中国矿业大学(北京) | Method for recovering furfural from furfural refining tower bottoms |
| CN115140791A (en) * | 2022-06-06 | 2022-10-04 | 河南汇阳化工科技有限公司 | Device and process for recovering and extracting furfural from process wastewater |
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