CN112939856A - Method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater - Google Patents
Method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater Download PDFInfo
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- CN112939856A CN112939856A CN202011624045.8A CN202011624045A CN112939856A CN 112939856 A CN112939856 A CN 112939856A CN 202011624045 A CN202011624045 A CN 202011624045A CN 112939856 A CN112939856 A CN 112939856A
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- pyridinecarboxamide
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- IBBMAWULFFBRKK-UHFFFAOYSA-N picolinamide Chemical compound NC(=O)C1=CC=CC=N1 IBBMAWULFFBRKK-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000002351 wastewater Substances 0.000 title claims abstract description 73
- FFNVQNRYTPFDDP-UHFFFAOYSA-N 2-cyanopyridine Chemical compound N#CC1=CC=CC=N1 FFNVQNRYTPFDDP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229920005989 resin Polymers 0.000 claims abstract description 64
- 239000011347 resin Substances 0.000 claims abstract description 64
- 238000003795 desorption Methods 0.000 claims abstract description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 230000008929 regeneration Effects 0.000 claims abstract description 5
- 238000011069 regeneration method Methods 0.000 claims abstract description 5
- 238000007670 refining Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 230000014759 maintenance of location Effects 0.000 claims description 8
- 229920006395 saturated elastomer Polymers 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000002808 molecular sieve Substances 0.000 claims description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 4
- 230000001172 regenerating effect Effects 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 6
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 description 5
- 238000004064 recycling Methods 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 206010012601 diabetes mellitus Diseases 0.000 description 2
- NOESYZHRGYRDHS-UHFFFAOYSA-N insulin Chemical compound N1C(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(NC(=O)CN)C(C)CC)CSSCC(C(NC(CO)C(=O)NC(CC(C)C)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CCC(N)=O)C(=O)NC(CC(C)C)C(=O)NC(CCC(O)=O)C(=O)NC(CC(N)=O)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CSSCC(NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2C=CC(O)=CC=2)NC(=O)C(CC(C)C)NC(=O)C(C)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2NC=NC=2)NC(=O)C(CO)NC(=O)CNC2=O)C(=O)NCC(=O)NC(CCC(O)=O)C(=O)NC(CCCNC(N)=N)C(=O)NCC(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC(O)=CC=3)C(=O)NC(C(C)O)C(=O)N3C(CCC3)C(=O)NC(CCCCN)C(=O)NC(C)C(O)=O)C(=O)NC(CC(N)=O)C(O)=O)=O)NC(=O)C(C(C)CC)NC(=O)C(CO)NC(=O)C(C(C)O)NC(=O)C1CSSCC2NC(=O)C(CC(C)C)NC(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(N)CC=1C=CC=CC=1)C(C)C)CC1=CN=CN1 NOESYZHRGYRDHS-UHFFFAOYSA-N 0.000 description 2
- 244000144972 livestock Species 0.000 description 2
- 244000144977 poultry Species 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- -1 2-acylaminopyridine Chemical compound 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 102000004877 Insulin Human genes 0.000 description 1
- 108090001061 Insulin Proteins 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- ZHNUHDYFZUAESO-UHFFFAOYSA-N formamide Substances NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229940125396 insulin Drugs 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/81—Amides; Imides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention belongs to the field of chemical industry, and particularly relates to a method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater, which comprises the following steps: (1) pretreatment: decolorizing and filtering the 2-cyanopyridine wastewater containing 2-pyridinecarboxamide, and adjusting the pH value to obtain a standby solution; (2) adsorption: adsorbing the standby liquid by a macroporous adsorption resin column to obtain wastewater containing less than 100ppm of 2-pyridinecarboxamide, and performing biochemical treatment; (3) desorption and regeneration, and the macroporous adsorption resin can be repeatedly used. 4) Refining: concentrating and rectifying the high-concentration desorption solution obtained in the step (3) to obtain a 2-pyridinecarboxamide product, and mechanically applying the recovered alcohol solution to desorption; the low-concentration desorption liquid is used as the first desorption agent of the next batch, and the water desorption liquid is used in the production process. The purity of the recovered 2-pyridinecarboxamide is more than or equal to 98%, the recovery rate is higher than 99%, the additional value of the 2-pyridinecarboxamide is improved, and the production cost of the 2-cyanopyridine can be reduced.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater.
Background
2-pyridinecarboxamide, alternative name of chinese: picolinamide, 2-acylaminopyridine, 2-picolinamide, pyridine-2-carboxamide, english name: pyridine-2-carboxamide, molecular formula and molecular weight: c6H6N2O122.12, appearance: off-white or off-white powder, melting point: 110 ℃ (dec.) (lit.), boiling point: 143 ℃/20 mmHg.
The 2-pyridine carboxamide is an important organic synthesis intermediate, is used for synthesizing various amide and ester derivatives in the medical industry, and has large market demand. It is also a synthetic raw material of many 2-pyridinecarboxamide salts, and has very wide application. For example, the 2-chromium picolinamide is one of the effective components in health food, not only can reduce the blood sugar level of a diabetic patient and the drug resistance of insulin, prevent and assist in treating diabetes, but also can play a role in preventing cardiovascular and cerebrovascular diseases. Meanwhile, the additive can be used as a feed additive for livestock and poultry to accelerate the growth and development of the livestock and poultry. The 2-pyridine carboxamide is also an important chemical auxiliary agent, is an important corrosion inhibition inhibitor, and can also be used as a light stabilizer of light-sensitive synthetic resin.
The prior patent introduces a process for treating and recycling picoline wastewater: adding the wastewater containing the picoline into a reaction kettle, adding a certain amount of flake caustic soda, starting stirring, stopping stirring after the flake caustic soda is completely melted, standing for layering, opening a kettle bottom valve of the reaction kettle, discharging a water layer at the bottom, and collecting the picoline at the upper layer and then sending the picoline to a rectification unit for recycling.
The documents and patents that employ the above methods are as follows: 1. guoqin, Tritifen, Yizajg, etc., a process for treating and recovering wastewater containing methylpyridine [ P ]. CN:108862862A.2018-11-23.
At present, the prior art does not provide a method for recovering 2-pyridinecarboxamide from waste water generated by 2-cyanopyridine, and the method fills up the technical blank of the method for recovering 2-pyridinecarboxamide from waste water generated by 2-cyanopyridine.
Disclosure of Invention
The invention aims to provide a method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater, wherein the wastewater in the 2-cyanopyridine production process contains a certain amount of 2-pyridinecarboxamide, and suspended matters or macromolecular tar and other impurities in the wastewater are removed through pretreatment; the pre-treated water adopts nonpolar or weak polar macroporous resin, and 2-pyridine formamide is intercepted through a macroporous net structure and a larger specific surface area of the macroporous resin. The invention adopts the macroporous adsorption resin technology to separate and recover the 2-pyridinecarboxamide in the wastewater, thereby realizing the resource recycling of the 2-pyridinecarboxamide and reducing the production cost of the 2-cyanopyridine.
The technical scheme of the invention is as follows:
a method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater comprises the following steps:
(1) pretreatment: decolorizing and filtering 2-cyanopyridine wastewater containing 2-pyridinecarboxamide to obtain a clear solution, and adjusting the pH value to 5-10 by using liquid alkali to obtain a standby solution;
(2) adsorption: adsorbing the standby liquid from bottom to top at the flow rate of 0.5-10 BV/h at normal temperature by using a macroporous adsorption resin column, controlling the retention time to be 0.1-2h, obtaining wastewater containing less than 100ppm of 2-pyridinecarboxamide, and performing biochemical treatment;
(3) desorption and regeneration: adsorbing the saturated resin in the step (1), discharging wastewater in the resin column, desorbing the resin column from top to bottom by using 45-95 mass percent of alcohol at a flow rate of 0.5-2 BV/h in a reverse direction for 1-4 h, collecting desorption liquid, and controlling the desorption temperature to be 30-60 ℃; washing the resin washed by alcohol with water, and desorbing and regenerating the macroporous adsorption resin for repeated use;
(4) refining: concentrating and rectifying the high-concentration desorption solution obtained in the step (3) to obtain a 2-pyridinecarboxamide product, and mechanically applying the recovered alcohol solution to desorption; the low-concentration desorption liquid is used as the first desorption agent of the next batch, and the water desorption liquid is used in the production process.
Further, in the step (2), the ratio of the height to the diameter of the resin column of the macroporous adsorption resin column is 3-15, and the resin column is one of D101 type, H-30 type, H-50 type, XDA-1G and molecular sieve.
Furthermore, in the step (2), the height-diameter ratio of the resin column of the macroporous adsorption resin column is 8-10.
And (3) further, adsorbing the standby liquid in the step (2) from bottom to top at the flow rate of 2-3 BV/h at normal temperature by using a macroporous adsorption resin column.
Further, the standby liquid in the step (2) is adsorbed on a macroporous adsorption resin column for 20min-1 h.
Further, in the step (3), the alcohol is one of methanol, ethanol and isopropanol.
According to the method for recovering 2-picolinamide from 2-cyanopyridine waste water, the concentration of the 2-cyanopyridine waste water containing 2-picolinamide is 2000-3000 ppm.
According to the method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater, in the step (1), the alkali is one of sodium hydroxide, potassium hydroxide and sodium carbonate.
The invention provides a method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater, which specifically comprises the following steps:
(1) pretreatment: decolorizing and filtering 2-cyanopyridine wastewater containing 2000-3000 ppm of 2-pyridinecarboxamide with activated carbon to obtain clear liquid, and adjusting the pH value to 5-10 with liquid alkali to obtain standby liquid;
(2) adsorption: adsorbing the standby liquid from bottom to top at the flow rate of 0.5-10 BV/H at normal temperature by using a macroporous adsorption resin column (the height-diameter ratio of the resin column is 3-15, one of D101 type, H-30 type, H-50 type, XDA-1G and a molecular sieve), controlling the retention time for 0.1-2H, obtaining wastewater containing less than 100ppm of 2-pyridinecarboxamide, and performing biochemical treatment;
(3) desorption and regeneration: adsorbing the saturated resin in the step (1), after the wastewater in the resin column is discharged, passing the resin column through a macroporous adsorption resin column from top to bottom in a reverse direction at a flow rate of 0.5-2 BV/h by using 45-95% of alcohol (mass percent of aqueous solution of a desorption agent, wherein the alcohol is one of methanol, ethanol and isopropanol), desorbing for 1-4 h, collecting desorption liquid, and controlling the desorption temperature to be 30 ℃
60 ℃; the resin washed by alcohol is washed by water again, and the macroporous adsorption resin can be repeatedly used after desorption and regeneration.
(4) Refining: concentrating and rectifying the high-concentration desorption solution obtained in the step (3) to obtain a 2-pyridinecarboxamide product, and mechanically applying the recovered alcohol solution to desorption; the low-concentration desorption liquid is used as the first desorption agent of the next batch, and the water desorption liquid is used in the production process.
Has the advantages that:
1) the invention has simple equipment, large treatment capacity and high automation degree, and is suitable for industrial continuous treatment; the whole process is continuously operated for 24 hours, and people are basically not required to directly participate in the operation;
2) the recovery rate of the 2-pyridinecarboxamide is high, the recovery rate is more than 99%, and the biodegradability of the wastewater is improved;
3) the purity of the recovered 2-pyridinecarboxamide is more than or equal to 98 percent, the recovery rate is more than 99 percent, the recovered 2-pyridinecarboxamide can be used for preparing downstream products, the additional value of the 2-pyridinecarboxamide can be improved, and the production cost of the 2-cyanopyridine can be reduced.
Drawings
FIG. 1 is a process flow diagram of a process for recovering 2-pyridinecarboxamide from 2-cyanopyridine waste water.
Detailed Description
The present invention is further illustrated below with reference to examples, which are understood by those skilled in the art to be illustrative only and not to constitute any limitation to the present invention.
Example 1: method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater
Decolorizing and filtering the wastewater containing 2000-3000 ppm of 2-pyridinecarboxamide, adjusting the pH to 5 by using liquid alkali, passing through a D101 type resin adsorption column (the height-diameter ratio is 12) from bottom to top at the flow rate of 0.5BV/h at normal temperature, and controlling the retention time of the wastewater on the adsorption resin for 2h to obtain the wastewater containing less than 100ppm of 2-pyridinecarboxamide. Adsorbing the saturated resin, discharging the wastewater in the resin, reversely desorbing the resin column from top to bottom by using 95% ethanol aqueous solution at the flow rate of 0.5BV/h, controlling the desorption temperature to be 30 ℃, and desorbing for 4 h. And concentrating, rectifying and separating the desorption solution, recovering ethanol for desorption and reuse, and obtaining the 2-pyridinecarboxamide with the purity of 98.1 percent, wherein the recovery rate of the 2-pyridinecarboxamide in the wastewater is 99.2 percent.
Example 2: method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater
The wastewater containing 2000-3000 ppm of 2-pyridinecarboxamide is decolored and filtered, the pH value is adjusted to 7 by liquid alkali, the wastewater passes through an H-30 type resin adsorption column (the height-diameter ratio is 8) from bottom to top at the flow rate of 2BV/H at normal temperature, the retention time of the wastewater on the adsorption resin is controlled for 1H, and the wastewater containing less than 100ppm of 2-pyridinecarboxamide is obtained. Adsorbing saturated resin, discharging wastewater in the resin, reversely desorbing the resin column from top to bottom by using 75% methanol aqueous solution at the flow rate of 1BV/h, controlling the desorption temperature to be 40 ℃, and desorbing for 2 h. And concentrating, rectifying and separating the desorption solution, recovering ethanol for desorption and reuse, and obtaining 98.2% of 2-pyridinecarboxamide, wherein the recovery rate of the 2-pyridinecarboxamide in the wastewater is 99.1%.
Example 3: method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater
Decolorizing and filtering the wastewater containing 2000-3000 ppm of 2-pyridinecarboxamide, adjusting the pH to 9 with liquid alkali, passing through an XDA-1G type resin adsorption column (the height-diameter ratio is 3) from bottom to top at the flow rate of 4BV/h at normal temperature, and controlling the retention time of the wastewater on the adsorption resin for 0.5h to obtain the wastewater containing less than 100ppm of 2-pyridinecarboxamide. Adsorbing the saturated resin, discharging the wastewater in the resin, reversely desorbing the resin column from top to bottom by 55 percent ethanol aqueous solution at the flow rate of 2BV/h, controlling the desorption temperature to be 60 ℃, and desorbing for 1 h. And concentrating, rectifying and separating the desorption solution, recovering ethanol for desorption and reuse, and obtaining 98.11% of 2-pyridinecarboxamide, wherein the recovery rate of the 2-pyridinecarboxamide in the wastewater is 99.2%.
Example 4: method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater
The wastewater containing 2000-3000 ppm of 2-pyridinecarboxamide is decolored and filtered, the pH value is adjusted to 10 by liquid alkali, the wastewater passes through a molecular sieve resin adsorption column (the height-diameter ratio is 12) from bottom to top at the flow rate of 6BV/h at normal temperature, the retention time of the wastewater on the adsorption resin is controlled for 10min, and the wastewater containing less than 100ppm of 2-pyridinecarboxamide is obtained. Adsorbing saturated resin, discharging wastewater in the resin, reversely desorbing the resin column from top to bottom by 55 percent isopropanol aqueous solution at the flow rate of 2BV/h, controlling the desorption temperature to be 60 ℃, and desorbing for 1 h. And concentrating, rectifying and separating the desorption solution, recovering ethanol for desorption and reuse, and obtaining 98.15% of 2-pyridinecarboxamide, wherein the recovery rate of the 2-pyridinecarboxamide in the wastewater is 99.1%.
Example 5: method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater
The wastewater containing 2000-3000 ppm of 2-pyridinecarboxamide is decolored and filtered, the pH value is adjusted to 7 by liquid alkali, the wastewater passes through an H-50 type resin adsorption column (the height-diameter ratio is 10) from bottom to top at the flow rate of 3BV/H at normal temperature, the retention time of the wastewater on the adsorption resin is controlled for 20min, and the wastewater containing less than 100ppm of 2-pyridinecarboxamide is obtained. Adsorbing the saturated resin, discharging the wastewater in the resin, reversely desorbing the resin column from top to bottom by using 85% ethanol aqueous solution at the flow rate of 2BV/h, controlling the desorption temperature to be 50 ℃, and desorbing for 1 h. And concentrating, rectifying and separating the desorption solution, recovering ethanol for desorption and reuse, and obtaining 98.2% of 2-pyridinecarboxamide, wherein the recovery rate of the 2-pyridinecarboxamide in the wastewater is 99.2%.
Claims (8)
1. A method for recovering 2-pyridinecarboxamide in 2-cyanopyridine wastewater is characterized by comprising the following steps:
(1) pretreatment: decolorizing and filtering 2-cyanopyridine wastewater containing 2-pyridinecarboxamide to obtain a clear solution, and adjusting the pH value to 5-10 to obtain a standby solution;
(2) adsorption: adsorbing the standby liquid from bottom to top at the flow rate of 0.5-10 BV/h at normal temperature by using a macroporous adsorption resin column, controlling the retention time to be 0.1-2h, obtaining wastewater containing less than 100ppm of 2-pyridinecarboxamide, and performing biochemical treatment;
(3) desorption and regeneration: adsorbing the saturated resin in the step (1), discharging wastewater in the resin column, desorbing the resin column from top to bottom by using 45-95 mass percent of alcohol at a flow rate of 0.5-2 BV/h in a reverse direction for 1-4 h, collecting desorption liquid, and controlling the desorption temperature to be 30-60 ℃; washing the resin washed by alcohol with water, and desorbing and regenerating the macroporous adsorption resin for repeated use;
(4) refining: concentrating and rectifying the high-concentration desorption solution obtained in the step (3) to obtain a 2-pyridinecarboxamide product, and mechanically applying the recovered alcohol solution to desorption; the low-concentration desorption liquid is used as the first desorption agent of the next batch, and the water desorption liquid is used in the production process.
2. The method for recovering 2-pyridinecarboxamide from 2-cyanopyridine wastewater according to claim 1,
in the step (2), the height-diameter ratio of the resin column of the macroporous adsorption resin column is 3-15, and the resin column is one of D101 type, H-30 type, H-50 type, XDA-1G and molecular sieve.
3. The method for recovering 2-pyridinecarboxamide from 2-cyanopyridine wastewater according to claim 1,
in the step (2), the height-diameter ratio of the resin column of the macroporous adsorption resin column is 8-10.
4. The method for recovering 2-pyridinecarboxamide from 2-cyanopyridine wastewater according to claim 1,
and (3) adsorbing the standby liquid in the step (2) from bottom to top at the normal temperature at the flow rate of 2-3 BV/h by using a macroporous adsorption resin column.
5. The method for recovering 2-pyridinecarboxamide from 2-cyanopyridine wastewater according to claim 1,
and (3) adsorbing the standby liquid in the step (2) for 20min-1h in a macroporous adsorption resin column.
6. The method for recovering 2-pyridinecarboxamide from 2-cyanopyridine waste water according to claim 1, wherein in step (3), the alcohol is one of methanol, ethanol, and isopropanol.
7. The method for recovering 2-pyridinecarboxamide in 2-cyanopyridine waste water according to claim 1, wherein the concentration of the 2-cyanopyridine waste water containing 2-pyridinecarboxamide is 2000-3000 ppm.
8. The method for recovering 2-pyridinecarboxamide from 2-cyanopyridine wastewater according to claim 1, wherein the alkali in step (1) is one of sodium hydroxide, potassium hydroxide, and sodium carbonate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114853243A (en) * | 2022-05-19 | 2022-08-05 | 山东潍坊润丰化工股份有限公司 | Recycling treatment method for 1,2,3, 6-tetrahydrophthalimide production wastewater |
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| CN114853243A (en) * | 2022-05-19 | 2022-08-05 | 山东潍坊润丰化工股份有限公司 | Recycling treatment method for 1,2,3, 6-tetrahydrophthalimide production wastewater |
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