CN110684023A - Method for recovering and separating thiamine mother liquor in caprolactam production process - Google Patents
Method for recovering and separating thiamine mother liquor in caprolactam production process Download PDFInfo
- Publication number
- CN110684023A CN110684023A CN201810727541.2A CN201810727541A CN110684023A CN 110684023 A CN110684023 A CN 110684023A CN 201810727541 A CN201810727541 A CN 201810727541A CN 110684023 A CN110684023 A CN 110684023A
- Authority
- CN
- China
- Prior art keywords
- tower kettle
- mother liquor
- separating
- recovering
- thiamine
- 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.)
- Pending
Links
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- JZRWCGZRTZMZEH-UHFFFAOYSA-N Thiamine Natural products CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N JZRWCGZRTZMZEH-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 235000019157 thiamine Nutrition 0.000 title claims abstract description 24
- 239000011721 thiamine Substances 0.000 title claims abstract description 24
- 239000012452 mother liquor Substances 0.000 title claims abstract description 23
- KYMBYSLLVAOCFI-UHFFFAOYSA-N thiamine Chemical compound CC1=C(CCO)SCN1CC1=CN=C(C)N=C1N KYMBYSLLVAOCFI-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229960003495 thiamine Drugs 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 17
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000010865 sewage Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract description 4
- 238000011084 recovery Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000000295 fuel oil Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000002920 hazardous waste Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 150000003544 thiamines Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D417/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00
- C07D417/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00 containing two hetero rings
- C07D417/06—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00 containing two hetero rings linked by a carbon chain containing only aliphatic carbon atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The method for recovering and separating thiamine mother liquor in the caprolactam production process is characterized by comprising the following steps: the method comprises the following steps: the method comprises the following steps: the thiamine mother liquor is conveyed to a preheater through a conveying pump for preheating, then enters an evaporator for evaporation, and is condensed and enters a collection tank and then is pumped into a sewage treatment system; evaporating the thiamine mother liquor to form tower kettle materials, feeding the tower kettle materials into a tower kettle receiving tank, and performing subsequent treatment; step two: controlling the tower kettle to pump the tower kettle materials into the stirring kettle through a tower kettle pump at 70 ℃, and simultaneously adding the organic solvent, wherein the tower kettle materials and the organic solvent are in a proportion of 3: 1, thereby precipitating the ammonium sulfate salt; step three: separating solid from liquid by a centrifugal machine, and adding a cleaning solvent at the same time according to the proportion of 6: 1, washing, drying the centrifuged and clean ammonium sulfate salt, and completing the recovery and separation.
Description
Technical Field
The invention belongs to the field of resource recovery, and particularly relates to a method for recovering and separating thiamine mother liquor in a caprolactam production process.
Background
The mother liquor containing thiamine is used as hazardous waste to be incinerated, a plurality of high value-added components in the residual liquid are not effectively utilized and are burnt, and simultaneously, due to the fact that the content of thiamine in the residual liquid is high, blockage of equipment and pipelines is caused in the incineration process, and due to the fact that the calorific value is low, a large amount of fuel oil is needed for combustion supporting, resource waste and environmental pollution are caused.
Disclosure of Invention
In order to solve the problems, the invention provides a method for recovering and separating thiamine mother liquor in a caprolactam production process.
The method for recovering and separating thiamine mother liquor in the caprolactam production process is characterized by comprising the following steps:
the method comprises the following steps:
the method comprises the following steps: the thiamine mother liquor is conveyed to a preheater through a conveying pump for preheating, then enters an evaporator for evaporation, and is condensed and enters a collection tank and then is pumped into a sewage treatment system; evaporating the thiamine mother liquor to form tower kettle materials, feeding the tower kettle materials into a tower kettle receiving tank, and performing subsequent treatment;
step two: controlling the tower kettle to pump the tower kettle materials into the stirring kettle through a tower kettle pump at 70 ℃, and simultaneously adding the organic solvent, wherein the tower kettle materials and the organic solvent are in a proportion of 3: 1, thereby precipitating the ammonium sulfate salt;
step three: separating solid from liquid by a centrifugal machine, and adding a cleaning solvent at the same time according to the proportion of 6: 1, washing, drying the centrifuged and clean ammonium sulfate salt, and completing the recovery and separation.
Further, the evaporation temperature of the evaporator was constant at 80 ℃.
Further, the preheating temperature of the preheater is 60 ℃.
And further, in the third step, the drying temperature is 100 ℃, and the drying time is 30 minutes.
The beneficial effects are as follows: the ammonium sulfate salt is extracted from the thiamine-containing mother liquor, the product reaches the industrial or agricultural ammonium sulfate salt standard, meanwhile, due to the fact that 30% of internal water is removed from the mother liquor and enters a sewage treatment system because of the purification of the ammonium sulfate salt, only other organic matters are left, the heat value is high, fuel oil does not need to be added for combustion supporting, and the waste of resources is reduced. The method has the advantages that the treatment of the environment is greatly improved, the environmental emission is reduced, the economic benefit is increased, the original hazardous waste is changed into comprehensive utilization from incineration disposal, the product yield of thiamine is increased, and the heat value of fuel oil is improved.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
A method for recovering and separating thiamine mother liquor in the production process of caprolactam,
1. removing water
Because the materials contain 30% of water, and the ammonium sulfate salt, caprolactam and caprolactam oligomer are all water-soluble, the water is removed firstly for separation, thiamine mother liquor is conveyed to a preheater E0102 through a P0101 conveying pump for preheating to 60 ℃, and then enters a film evaporator, the temperature of the film evaporator is controlled to be 80 ℃, materials at the top of the tower are water vapor, the water vapor is condensed and enters a sewage collecting tank and then is conveyed to a sewage treatment system, and materials at the bottom of the tower enter a receiving tank V0101 at the bottom of the tower and enter subsequent treatment.
Dissolving and stirring
And after dehydration, the fluidity of the bottom material is poor, the temperature of the tower kettle is controlled to be 70 ℃, the bottom material is pumped into the stirring kettle through a tower kettle pump, and an organic solvent is added according to the proportion of 3: 1, changing the fluidity, according to the similarity solution principle, dissolving caprolactam and oligomer in organic matter, and precipitating ammonium sulfate in the lower layer for phase separation.
Centrifugal filtration
And (3) separating solid from liquid by a centrifugal machine, and simultaneously adding a cleaning solvent for controlling high-content thiamine salt according to the ratio of 6: 1, washing, drying the centrifuged and cleaned ammonium sulfate salt, controlling the temperature at 100 ℃, and drying for less than half an hour to obtain the ammonium sulfate salt product.
The ammonium sulfate salt is extracted from the thiamine-containing mother liquor, the product reaches the industrial or agricultural ammonium sulfate salt standard, meanwhile, due to the fact that 30% of internal water is removed from the mother liquor and enters a sewage treatment system because of the purification of the ammonium sulfate salt, only other organic matters are left, the heat value is high, fuel oil does not need to be added for combustion supporting, and the waste of resources is reduced. The method has the advantages that the treatment of the environment is greatly improved, the environmental emission is reduced, the economic benefit is increased, the original hazardous waste is changed into comprehensive utilization from incineration disposal, the product yield of thiamine is increased, and the heat value of fuel oil is improved.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (4)
1. The method for recovering and separating thiamine mother liquor in the caprolactam production process is characterized by comprising the following steps:
the method comprises the following steps:
the method comprises the following steps: the thiamine mother liquor is conveyed to a preheater through a conveying pump for preheating, then enters an evaporator for evaporation, and is condensed and enters a collection tank and then is pumped into a sewage treatment system; evaporating the thiamine mother liquor to form tower kettle materials, feeding the tower kettle materials into a tower kettle receiving tank, and performing subsequent treatment;
step two: controlling the tower kettle to pump the tower kettle materials into the stirring kettle through a tower kettle pump at 70 ℃, and simultaneously adding the organic solvent, wherein the tower kettle materials and the organic solvent are in a proportion of 3: 1, thereby precipitating the ammonium sulfate salt;
step three: separating solid from liquid by a centrifugal machine, and adding a cleaning solvent at the same time according to the proportion of 6: 1, washing, drying the centrifuged and clean ammonium sulfate salt, and completing the recovery and separation.
2. The process for recovering and separating thiamin mother liquor from caprolactam production according to claim 1, wherein: the evaporation temperature of the evaporator was constant at 80 ℃.
3. The process for recovering and separating thiamin mother liquor from caprolactam production according to claim 1, wherein: the preheating temperature of the preheater is 60 ℃.
4. The process for recovering and separating thiamin mother liquor from caprolactam production according to claim 1, wherein: in the third step, the drying temperature is 100 ℃, and the drying time is 30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810727541.2A CN110684023A (en) | 2018-07-05 | 2018-07-05 | Method for recovering and separating thiamine mother liquor in caprolactam production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810727541.2A CN110684023A (en) | 2018-07-05 | 2018-07-05 | Method for recovering and separating thiamine mother liquor in caprolactam production process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110684023A true CN110684023A (en) | 2020-01-14 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810727541.2A Pending CN110684023A (en) | 2018-07-05 | 2018-07-05 | Method for recovering and separating thiamine mother liquor in caprolactam production process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110684023A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538548A (en) * | 2022-02-25 | 2022-05-27 | 苏州仕净科技股份有限公司 | Low-cost ammonium sulfate waste liquid recycling treatment process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1254711A (en) * | 1998-11-19 | 2000-05-31 | 巴陵石化鹰山石油化工厂 | Process for recovering useful substances from waste liquid generated in preparing process of caprolactam |
| CN101049980A (en) * | 2007-05-23 | 2007-10-10 | 徐明光 | Method for comprehensive utilization for benzene extracting concentrated solution of residue wastewater |
-
2018
- 2018-07-05 CN CN201810727541.2A patent/CN110684023A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1254711A (en) * | 1998-11-19 | 2000-05-31 | 巴陵石化鹰山石油化工厂 | Process for recovering useful substances from waste liquid generated in preparing process of caprolactam |
| CN101049980A (en) * | 2007-05-23 | 2007-10-10 | 徐明光 | Method for comprehensive utilization for benzene extracting concentrated solution of residue wastewater |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538548A (en) * | 2022-02-25 | 2022-05-27 | 苏州仕净科技股份有限公司 | Low-cost ammonium sulfate waste liquid recycling treatment process |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: No.157 puqiao Road, Nanjing Chemical Industrial Park, Nanjing, Jiangsu 210000 Applicant after: Nanjing Changjiang Jiangyu Environmental Protection Technology Co.,Ltd. Address before: No.157 puqiao Road, Nanjing Chemical Industrial Park, Nanjing, Jiangsu 210000 Applicant before: NANJING CHANGJIANG JIANGYU PETROCHEMICAL Co.,Ltd. |
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| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20200114 |