CN112479919A - Method for recovering dilute DMF (dimethyl formamide) in sucralose crystallization mother liquor wastewater - Google Patents
Method for recovering dilute DMF (dimethyl formamide) in sucralose crystallization mother liquor wastewater Download PDFInfo
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- CN112479919A CN112479919A CN202011367835.2A CN202011367835A CN112479919A CN 112479919 A CN112479919 A CN 112479919A CN 202011367835 A CN202011367835 A CN 202011367835A CN 112479919 A CN112479919 A CN 112479919A
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- octanol
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- 239000002351 wastewater Substances 0.000 title claims abstract description 60
- 239000012452 mother liquor Substances 0.000 title claims abstract description 22
- 238000002425 crystallisation Methods 0.000 title claims abstract description 20
- 230000008025 crystallization Effects 0.000 title claims abstract description 20
- 239000004376 Sucralose Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 title claims abstract description 17
- 235000019408 sucralose Nutrition 0.000 title claims abstract description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 title abstract description 127
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims abstract description 76
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 239000012074 organic phase Substances 0.000 claims abstract description 20
- 239000010865 sewage Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000012071 phase Substances 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012528 membrane Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000011084 recovery Methods 0.000 claims abstract description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000284 extract Substances 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 4
- 239000000126 substance Substances 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- NGDNVOAEIVQRFH-UHFFFAOYSA-N 2-nonanol Chemical compound CCCCCCCC(C)O NGDNVOAEIVQRFH-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 230000003203 everyday effect Effects 0.000 description 2
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 2
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method for recovering diluted DMF (dimethyl formamide) in sucralose crystallization mother liquor wastewater, which is characterized by comprising the following steps of: (1) sending the wastewater into a membrane filter press for filtering to remove solid impurities; (2) conveying the filtered wastewater into an extraction tower at a speed of 8-10m for carrying out thin-wall ethanol distillation/h, adding n-octanol into the extraction tower at a speed of 8-10m for carrying out thin-wall ethanol distillation/h, fully mixing, standing for layering, directly conveying a water phase out of a sewage station after layering, and conveying an organic phase into an intermediate tank; (3) and sending the organic phase into a rectifying tower for reduced pressure distillation at the speed of 8-10 m/h, controlling the bottom pressure of the rectifying tower to be-0.09 to-0.1 MPa, the temperature to be 101-: 1, externally sending the extracted substances at the top of the tower to a recovery working section, and sending n-octanol extracted at the bottom of the tower to an intermediate tank at the front section of extraction after heat exchange with a feeding organic phase of a rectifying tower, and applying the n-octanol to the extracting tower. The invention has the beneficial effects that: the high-temperature waste water can be directly used for extraction, so that the energy consumption is saved; 3-4% of DMF in the wastewater is enriched into 9-11% of DMF, and 10t/d of DMF can be stably recovered.
Description
Technical Field
The invention belongs to the field of food additive production, and relates to a method for recovering diluted DMF (dimethyl formamide) in sucralose crystallization mother liquor wastewater.
Background
In the production of sucralose, after the neutralization solution is concentrated and dried, decoloring and crystallizing are carried out, wherein mother liquor generated in the crystallization process contains ethyl acetate and waste water, and after the mother liquor is kept stand for layering to remove ethyl acetate, the waste water also contains low-concentration (3-4%) DMF. In the current production, the wastewater is produced by about 300m each day, the existing treatment method is to directly discharge the part of wastewater, and when sewage is treated, DMF loss is caused by 9-12 tons/day; and the DMF has stable property and poor biodegradability, is easy to kill bacterial colonies, and a large amount of DMF is used for a sewage treatment system, so that the load of the sewage treatment system is increased, and the treatment cost is increased.
Disclosure of Invention
The invention aims to solve the problems that after ethyl acetate is removed by layering of sucralose crystallization mother liquor, residual wastewater (containing 3-4% of DMF) is directly discharged, DMF loss is caused, the load of a sewage treatment system is increased, and the treatment cost is high and high, and provides a method for recovering diluted DMF from sucralose crystallization mother liquor wastewater.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for recovering diluted DMF in sucralose crystallization mother liquor wastewater is characterized by comprising the following steps:
(1) feeding the wastewater (the wastewater obtained after ethyl acetate is removed from crystallization mother liquor by layering at 5-10 ℃ and DMF 3-4%) into a membrane filter press for filtering to remove solid impurities in the wastewater;
(2) conveying the filtered wastewater (65-75 ℃) into an extraction tower at the rate of 8-10m for carrying out thin film chromatography, adding n-octanol into the extraction tower at the rate of 8-10m for carrying out thin film chromatography, fully mixing, standing for layering, directly conveying a layered water phase to a sewage station, and conveying an organic phase (7-9% of water, 2-4% of DMF and 85-88% of n-octanol) into an intermediate tank;
(3) and (2) conveying the organic phase in the middle groove into a rectifying tower for reduced pressure distillation in an amount of 8-10 m/h, controlling the bottom pressure of the rectifying tower to be-0.09-0.1 MPa, the temperature to be 101-: 1, delivering a product (containing DMF 9-11%) extracted from the top of the rectifying tower to a recovery working section (DMF dehydration tower), exchanging heat between n-octanol (the n-octanol is more than or equal to 99%) extracted from the bottom of the rectifying tower and a feeding organic phase of the rectifying tower, delivering the n-octanol to an intermediate tank at the front section of extraction, and applying the n-octanol to the extraction tower.
The method selects n-octanol as an extracting agent, utilizes the n-octanol to have good extraction efficiency and selectivity on low-concentration DMF wastewater, extracts the low-concentration DMF, enters an extracted organic phase into a decompression rectifying tower to be rectified to obtain the n-octanol and relatively pure dilute DMF (9-11%), and removes sewage from a raffinate phase to serve as wastewater treatment; and n-octanol extracted from the bottom of the rectifying tower is applied to the extraction tower, DMF extracted from the top of the rectifying tower and the water jacket are used in a DMF dehydration tower of an alcoholysis workshop for dehydration, and then rectification is performed.
The invention has the beneficial effects that:
1. the invention does not need to carry out cooling treatment on the wastewater, can directly utilize high-temperature (65-75 ℃) wastewater for extraction, and saves a large amount of energy consumption;
2. recovering 3-4% of dilute DMF in the wastewater to enrich the dilute DMF into 9-11% of high purity, stably recovering 10t/d of DMF, wherein the benefit created every day reaches 6 ten thousand yuan and the benefit created all the year round reaches 2190 ten thousand yuan according to 6000 yuan per ton price;
3. solid impurities in the wastewater are filtered and removed, so that the problem of pipe blockage in subsequent working sections can be effectively reduced, the difficulty of sewage treatment is reduced after DMF in the wastewater is recovered, and the risk of fungus death is reduced;
4. in the invention, part of the wastewater is transferred to the n-octanol phase, then the water is evaporated in the rectifying tower, and finally the wastewater is applied to a decimetric system for producing ammonia water, so that the generation of 21 tons of high-ammonia nitrogen salt-containing wastewater is reduced every day, the treatment cost of each ton of high-ammonia nitrogen salt-containing wastewater is 2000 yuan, and the sewage treatment cost is saved and the cost is saved by 1520 ten thousand yuan all the year.
Drawings
FIG. 1 is a schematic diagram of a process for recovering dilute DMF from sucralose crystallization mother liquor wastewater.
Detailed Description
This episode is further explained in connection with fig. 1: a method for recovering diluted DMF in sucralose crystallization mother liquor wastewater comprises the following specific implementation steps:
example 1
(1) Conveying the 24 m wastewater (wastewater obtained after ethyl acetate is removed from crystallization mother liquor in a layering mode at 75 ℃ and 3.5% of DMF) into a membrane filter press for filtering to remove solid impurities in the wastewater;
(2) conveying the filtered wastewater (70 ℃) into an extraction tower according to the weight of 9m for carrying out thin film chromatography/h, adding n-octanol into the extraction tower according to the weight of 9m for carrying out thin film chromatography/h, fully mixing, standing for 30min for layering, directly conveying a layered water phase to a sewage station, and conveying an organic phase (water 7.5%, DMF 3.5%, n-octanol 87%, and the rest components are organic impurities) into an intermediate tank;
(3) and (3) carrying out reduced pressure distillation on the organic phase in the middle groove by the weight of 9 m/h in a rectifying tower, controlling the tower bottom pressure of the rectifying tower to be-0.09 MPa, the temperature to be 106 ℃, the tower top temperature of the rectifying tower to be 92 ℃, and the reflux ratio to be 0.8: and 1, carrying out 10m heavy planting on the extract at the top of the rectifying tower (containing DMF 10%) and conveying the extract to a recovery working section (DMF dehydration tower), carrying out heat exchange on n-octanol (99.5%) extracted at the bottom of the rectifying tower and a feeding organic phase of the rectifying tower, conveying the n-octanol to an intermediate tank at the front section of extraction, and mechanically applying the n-octanol to the extraction tower.
Example 2
(1) Conveying the 20m wastewater (wastewater obtained after ethyl acetate is removed from crystallization mother liquor in a layering mode, 65 ℃ and 3 percent of DMF) into a membrane filter press for filtering to remove solid impurities in the wastewater;
(2) conveying the filtered wastewater (60 ℃) into an extraction tower at the rate of 8.2 m/h, adding n-octanol into the extraction tower at the rate of 8.2 m/h, fully mixing, standing for 25min for layering, directly conveying a layered water phase to a sewage station, and conveying an organic phase (8% of water, 3% of DMF, 87% of n-octanol, and the rest components are organic impurities) into an intermediate tank;
(3) and (3) conveying the organic phase in the middle groove into a rectifying tower for reduced pressure distillation in an amount of 8.2 m/h, controlling the tower bottom pressure of the rectifying tower to be-0.07 MPa, the temperature to be 102 ℃, the tower top temperature of the rectifying tower to be 88 ℃, and the reflux ratio to be 0.6: 1, carrying out 10m heavy planting on the extract at the top of the rectifying tower (containing DMF 9%) and conveying the extract to a recovery working section (DMF dehydration tower), carrying out heat exchange on n-octanol (99.2%) extracted at the bottom of the rectifying tower and a feeding organic phase of the rectifying tower, conveying the n-octanol to an intermediate tank at the front section of extraction, and mechanically applying the n-octanol to the extraction tower.
Example 3
(1) Conveying the 30m wastewater (wastewater obtained after ethyl acetate is removed from crystallization mother liquor in a layering mode, the temperature is 70 ℃, and DMF 4%) into a membrane filter press for filtering to remove solid impurities in the wastewater;
(2) conveying the filtered wastewater (65 ℃) into an extraction tower in an amount of 10m for carrying out heavy year/h, adding n-octanol into the extraction tower in an amount of 10m for carrying out heavy year/h, fully mixing, standing for 40min for layering, directly conveying a layered water phase to a sewage station, and conveying an organic phase (water 7.8%, DMF 3.2%, n-octanol 87%, and the rest components are organic impurities) into an intermediate tank;
(3) and (3) carrying out reduced pressure distillation on the organic phase in the middle groove by 10 m/h, controlling the bottom pressure of the rectifying tower to be-0.05 MPa, the temperature to be 110 ℃, the top temperature of the rectifying tower to be 96 ℃, and the reflux ratio to be 1: and 1, carrying out 10m heavy planting on the extract at the top of the rectifying tower (containing DMF 11%) and conveying the extract to a recovery working section (DMF dehydration tower), carrying out heat exchange on n-octanol (99.7%) extracted at the bottom of the rectifying tower and a feeding organic phase of the rectifying tower, conveying the n-octanol to an intermediate tank at the front section of extraction, and mechanically applying the n-octanol to the extraction tower.
Description of the extractant and its effect: chloroform, n-octanol, isooctanol, nonanol, 2-nonanol and the like are selected preliminarily as extracting agents for carrying out comparison tests; taking the wastewater with the same volume, respectively adding the extracting agents with the same volume, oscillating for 3min in a separating funnel, standing for 30min for layering, and sampling to determine the concentration value of DMF in raffinate.
The distribution coefficient is represented by D as:
table one: the extraction efficiency of different extracting agents on DMF in sucralose wastewater is as follows:
table two: according to different n-octyl alcohol phases: the extraction rate obtained under the conditions of the wastewater phase proportion is as follows:
the following can be seen from the above tables: the n-octanol has the best extraction effect on low-concentration DMF in the wastewater, and the n-octanol: the extraction effect is ideal when the volume ratio of the waste water is between 1: 2.
Claims (6)
1. A method for recovering diluted DMF in sucralose crystallization mother liquor wastewater is characterized by comprising the following steps:
(1) sending the wastewater into a membrane filter press for filtering, and removing solid impurities in the wastewater;
(2) conveying the filtered wastewater into an extraction tower according to the weight of 8-10 m/h, adding n-octanol into the extraction tower according to the weight of 8-10 m/h, fully mixing, standing for layering, directly conveying the layered water phase to a sewage station, and conveying the organic phase to an intermediate tank;
(3) and (2) conveying the organic phase in the middle groove into a rectifying tower for reduced pressure distillation in an amount of 8-10 m/h, controlling the bottom pressure of the rectifying tower to be-0.09-0.1 MPa, the temperature to be 101-: 1, externally sending the extract at the top of the rectifying tower to a recovery working section, and sending n-octanol extracted at the bottom of the rectifying tower to an intermediate tank at the front section of extraction after heat exchange with a feeding organic phase of the rectifying tower, and applying the n-octanol to the extracting tower.
2. The method for recovering diluted DMF in the mother liquor wastewater of sucralose crystallization according to claim 1, which is characterized in that: the wastewater obtained in the step (1) is obtained by removing ethyl acetate from crystal mother liquor in a layering manner, the wastewater is 5-10 ℃, and the DMF content is 3-4%.
3. The method for recovering diluted DMF in the mother liquor wastewater of sucralose crystallization according to claim 1, which is characterized in that: the temperature of the filtered wastewater in the step (2) is 65-75 ℃.
4. The method for recovering diluted DMF in the mother liquor wastewater of sucralose crystallization according to claim 1, which is characterized in that: in the step (2), the organic phase contains 7-9% of water, 2-4% of DMF and 85-88% of n-octanol.
5. The method for recovering diluted DMF in the mother liquor wastewater of sucralose crystallization according to claim 1, which is characterized in that: the extract at the top of the rectifying tower in the step (3) contains 9-11% of DMF.
6. The method for recovering diluted DMF from sucralose crystallization mother liquor wastewater according to any one of claims 1 to 5, characterized in that: and (3) the n-octanol extracted from the bottom of the rectifying tower in the step (3) is not less than 99%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011367835.2A CN112479919A (en) | 2020-11-30 | 2020-11-30 | Method for recovering dilute DMF (dimethyl formamide) in sucralose crystallization mother liquor wastewater |
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| CN202011367835.2A CN112479919A (en) | 2020-11-30 | 2020-11-30 | Method for recovering dilute DMF (dimethyl formamide) in sucralose crystallization mother liquor wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112513007A (en) * | 2020-10-23 | 2021-03-16 | 安徽金禾实业股份有限公司 | DMF (dimethyl formamide) recovery method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1554676A (en) * | 1976-11-01 | 1979-10-24 | Mitsubishi Gas Chemical Co | Process for producing dimethylformamide |
| CN1793111A (en) * | 2005-11-04 | 2006-06-28 | 清华大学 | Process for recovering dimethyl formyl amide from waste water |
| CN101397260A (en) * | 2008-11-19 | 2009-04-01 | 河北工业大学 | Technology for recovering dimethylformamide from waste water by combination of saline extraction and rectification method |
| US20120289693A1 (en) * | 2011-05-10 | 2012-11-15 | Tate & Lyle Technology Limited | Extraction of Carboxylic Acids with Tin Compounds |
| CN111100028A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Extraction-rectification recovery method of N, N-dimethylformamide |
-
2020
- 2020-11-30 CN CN202011367835.2A patent/CN112479919A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1554676A (en) * | 1976-11-01 | 1979-10-24 | Mitsubishi Gas Chemical Co | Process for producing dimethylformamide |
| CN1793111A (en) * | 2005-11-04 | 2006-06-28 | 清华大学 | Process for recovering dimethyl formyl amide from waste water |
| CN101397260A (en) * | 2008-11-19 | 2009-04-01 | 河北工业大学 | Technology for recovering dimethylformamide from waste water by combination of saline extraction and rectification method |
| US20120289693A1 (en) * | 2011-05-10 | 2012-11-15 | Tate & Lyle Technology Limited | Extraction of Carboxylic Acids with Tin Compounds |
| CN111100028A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Extraction-rectification recovery method of N, N-dimethylformamide |
Non-Patent Citations (1)
| Title |
|---|
| 李春利 等: "正辛醇作为萃取剂回收废水中低浓度的DMF", 《现代化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112513007A (en) * | 2020-10-23 | 2021-03-16 | 安徽金禾实业股份有限公司 | DMF (dimethyl formamide) recovery method |
| CN112513007B (en) * | 2020-10-23 | 2022-01-21 | 安徽金禾实业股份有限公司 | DMF (dimethyl formamide) recovery method |
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Application publication date: 20210312 |