CN113461613A - Method for purifying isoquinoline - Google Patents
Method for purifying isoquinoline Download PDFInfo
- Publication number
- CN113461613A CN113461613A CN202110815736.4A CN202110815736A CN113461613A CN 113461613 A CN113461613 A CN 113461613A CN 202110815736 A CN202110815736 A CN 202110815736A CN 113461613 A CN113461613 A CN 113461613A
- Authority
- CN
- China
- Prior art keywords
- isoquinoline
- solution
- residual liquid
- crystals
- strong acid
- 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
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 title claims abstract description 210
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 83
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 150000002537 isoquinolines Chemical class 0.000 claims abstract description 38
- 230000035900 sweating Effects 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 30
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 29
- 239000003960 organic solvent Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000354 decomposition reaction Methods 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims 3
- 208000008454 Hyperhidrosis Diseases 0.000 abstract description 34
- 238000000746 purification Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- SYBYTAAJFKOIEJ-UHFFFAOYSA-N 3-Methylbutan-2-one Chemical compound CC(C)C(C)=O SYBYTAAJFKOIEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- -1 etc. Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D217/00—Heterocyclic compounds containing isoquinoline or hydrogenated isoquinoline ring systems
- C07D217/02—Heterocyclic compounds containing isoquinoline or hydrogenated isoquinoline ring systems with only hydrogen atoms or radicals containing only carbon and hydrogen atoms, directly attached to carbon atoms of the nitrogen-containing ring; Alkylene-bis-isoquinolines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to the field of purification, and discloses a method for purifying isoquinoline in order to solve the problem of poor purification effect of the existing method for purifying isoquinoline, which comprises the following raw materials: isoquinoline residual liquid, organic solvent, strong acid solution, ethanol solution and ammonia water solution. According to the method, firstly, strong acid is used for reacting with isoquinoline in the isoquinoline residual liquid to obtain isoquinoline residual liquid salt, then the isoquinoline in the isoquinoline salt is decomposed by ammonia water to obtain crude isoquinoline crystals, and then the crude isoquinoline crystals are subjected to three times of sweating treatment, so that impurities in the crude crystals are further melted and discharged, the purity of the isoquinoline crystals is improved, the purification effect is better, and the method is simple to operate, high in feasibility and easy to industrially control.
Description
Technical Field
The invention relates to the technical field of purification, in particular to a method for purifying isoquinoline.
Background
Isoquinoline is colorless crystal, can be mixed and dissolved with various organic solvents, and is dissolved in dilute acid; has water absorption and stronger alkalinity than quinoline, and is used for the production of products such as pesticide, medicine, rubber accelerator, color film sensitizer, dye, and the like. Used as raw materials of medicines, dyes, insecticides, anion exchange resins, etc., iron preservatives, curing agents for resol resins, etc.
At present, isoquinoline is extracted from coal tar mainly through a distillation crystallization method, and then is further purified and reused, but the existing isoquinoline purification method has the problem of poor purification effect.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for purifying isoquinoline.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for purifying isoquinoline, comprising the following steps:
step 1: according to the following steps of 60: (35-40): (10-18): (20-25): (5-15) weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio;
step 2: pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at the temperature of 30-40 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals;
and step 3: pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals;
and 4, step 4: carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 20-25 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 30-35 ℃; and (3) sweating the isoquinoline crystal for the third time in a constant temperature environment of 40-45 ℃ to obtain the isoquinoline crystal.
Preferably, the mass percentage of isoquinoline in the isoquinoline residual liquid is 35 to 85 percent.
Preferably, the organic solvent is one of methanol, ethanol, diethyl ether, toluene and methyl butanone.
Preferably, the strong acid solution is one of concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid.
Preferably, the concentration of the ethanol solution in the step 3 is 75-90%; the concentration of the ammonia solution is 18-30%.
Preferably, according to 60: (36-38): (12-16): (18-23): (6-14) weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio.
Preferably, according to 60: 37: 14: 22: weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio of 10.
Preferably, according to 60: (36.5-38.5): (13-15): (21.5-23): (9-11) weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio.
Preferably, the purity of the isoquinoline crystal obtained in the step 4 is 98-99.99%.
Preferably, the sweating time in step 4 is 0.5-1 h.
The invention has the beneficial effects that:
according to the method, firstly, strong acid is used for reacting with isoquinoline in the isoquinoline residual liquid to obtain isoquinoline residual liquid salt, then the isoquinoline in the isoquinoline salt is decomposed by ammonia water to obtain crude isoquinoline crystals, and then the crude isoquinoline crystals are subjected to three times of sweating treatment, so that impurities in the crude crystals are further melted and discharged, the purity of the isoquinoline crystals is improved, the purification effect is better, and the method is simple to operate, high in feasibility and easy to industrially control.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
Weighing 60 g of 35% by mass of isoquinoline residual liquid, 35 g of organic solvent, 10 g of strong acid solution, 20 g of 75% ethanol solution and 5 g of 18% ammonia water solution; pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at the temperature of 30 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals; pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals; carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 20 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 30 ℃; and (3) carrying out third sweating on the isoquinoline crystal in a constant temperature environment of 40 ℃, wherein the sweating time of each time is 0.5h, so as to obtain the isoquinoline crystal.
Example 2
Weighing 60 g of isoquinoline residual liquid with the mass percentage of 85%, 40 g of organic solvent, 18 g of strong acid solution, 25 g of ethanol solution with the concentration of 90% and 15 g of ammonia water solution with the concentration of 30%; pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at 40 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals; pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals; carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 25 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 35 ℃; and (3) carrying out third sweating on the isoquinoline crystal in a constant temperature environment of 45 ℃, wherein the sweating time of each time is 1h, so as to obtain the isoquinoline crystal.
Example 3
Weighing 60 g of isoquinoline residual liquid with the mass percentage of 85%, 38 g of organic solvent, 16 g of strong acid solution, 23 g of ethanol solution with the concentration of 90% and 14 g of ammonia water solution with the concentration of 30%; pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at 40 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals; pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals; carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 25 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 35 ℃; and (3) carrying out third sweating on the isoquinoline crystal in a constant temperature environment of 45 ℃, wherein the sweating time of each time is 1h, so as to obtain the isoquinoline crystal.
Example 4
Weighing 60 g of 35% by mass of isoquinoline residual liquid, 36 g of organic solvent, 12 g of strong acid solution, 18 g of 75% ethanol solution and 6 g of 18% ammonia water solution; pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at the temperature of 30 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals; pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals; carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 20 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 30 ℃; and (3) carrying out third sweating on the isoquinoline crystal in a constant temperature environment of 40 ℃, wherein the sweating time of each time is 0.5h, so as to obtain the isoquinoline crystal.
Example 5
Weighing 60 g of isoquinoline residual liquid with the mass percentage of 85%, 37 g of organic solvent, 14 g of strong acid solution, 22 g of ethanol solution with the concentration of 90% and 10 g of ammonia water solution with the concentration of 30%; pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at 40 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals; pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals; carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 25 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 35 ℃; and (3) carrying out third sweating on the isoquinoline crystal in a constant temperature environment of 45 ℃, wherein the sweating time of each time is 1h, so as to obtain the isoquinoline crystal.
Example 6
Weighing 60 g of 35 percent by mass of isoquinoline residual liquid, 36.5 g of organic solvent, 13 g of strong acid solution, 21.5 g of 75-90 percent ethanol solution and 9 g of 18 percent ammonia water solution; pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at the temperature of 30 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals; pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals; carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 20 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 30 ℃; and (3) carrying out third sweating on the isoquinoline crystal in a constant temperature environment of 40 ℃, wherein the sweating time of each time is 0.5h, so as to obtain the isoquinoline crystal.
Example 7
Weighing 60 g of isoquinoline residual liquid with the mass percentage of 85%, 38.5 g of organic solvent, 15 g of strong acid solution, 23 g of ethanol solution with the concentration of 90% and 11 g of ammonia water solution with the concentration of 30%; pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at 40 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals; pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals; carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 25 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 35 ℃; and (3) carrying out third sweating on the isoquinoline crystal in a constant temperature environment of 45 ℃, wherein the sweating time of each time is 1h, so as to obtain the isoquinoline crystal.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The method for purifying isoquinoline is characterized by comprising the following steps:
step 1: according to the following steps of 60: (35-40): (10-18): (20-25): (5-15) weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio;
step 2: pouring the isoquinoline residual liquid into an organic solvent and a strong acid solution, fully mixing at the temperature of 30-40 ℃ to obtain isoquinoline salt, and cooling and crystallizing to separate out isoquinoline salt crystals;
and step 3: pouring the isoquinoline salt crystals into an ethanol solution, mixing until the isoquinoline salt crystals are dissolved, adding an ammonia water solution, fully stirring for decomposition, and heating for dehydration to obtain crude isoquinoline crystals;
and 4, step 4: carrying out first sweating on the isoquinoline crystal in a constant temperature environment of 20-25 ℃; carrying out second sweating on the isoquinoline crystal in a constant temperature environment of 30-35 ℃; and (3) sweating the isoquinoline crystal for the third time in a constant temperature environment of 40-45 ℃ to obtain the isoquinoline crystal.
2. The method for purifying isoquinoline of claim 1, wherein the mass percentage of isoquinoline in the isoquinoline residual liquid is 35 to 85 percent.
3. The method of claim 1, wherein the organic solvent is one of methanol, ethanol, diethyl ether, toluene, and methyl ethyl ketone.
4. The method of claim 1, wherein the strong acid solution is one of concentrated sulfuric acid, concentrated hydrochloric acid, and concentrated nitric acid.
5. The method for purifying isoquinoline according to claim 1, wherein the concentration of the ethanol solution in the step 3 is 75 to 90%; the concentration of the ammonia solution is 18-30%.
6. The method of claim 1, wherein the ratio of 60: (36-38): (12-16): (18-23): (6-14) weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio.
7. The method of claim 1, wherein the ratio of 60: 37: 14: 22: weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio of 10.
8. The method of claim 1, wherein the ratio of 60: (36.5-38.5): (13-15): (21.5-23): (9-11) weighing isoquinoline residual liquid, an organic solvent, a strong acid solution, an ethanol solution and an ammonia water solution according to the weight ratio.
9. The method for purifying isoquinoline according to any one of claims 1 to 8, wherein the purity of the isoquinoline crystals obtained in step 4 is 98% to 99.99%.
10. The method for purifying isoquinoline in claim 1, wherein each sweating time in step 4 is 0.5 to 1 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110815736.4A CN113461613A (en) | 2021-07-19 | 2021-07-19 | Method for purifying isoquinoline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110815736.4A CN113461613A (en) | 2021-07-19 | 2021-07-19 | Method for purifying isoquinoline |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113461613A true CN113461613A (en) | 2021-10-01 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110815736.4A Pending CN113461613A (en) | 2021-07-19 | 2021-07-19 | Method for purifying isoquinoline |
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2483420A (en) * | 1946-03-08 | 1949-10-04 | Koppers Co Inc | Purification of isoquinoline |
| JPH0334970A (en) * | 1989-06-30 | 1991-02-14 | Kawasaki Steel Corp | Method for purifying isoquinoline |
| JPH04275275A (en) * | 1991-03-04 | 1992-09-30 | Nippon Steel Chem Co Ltd | Recovery of isoquinoline and quinaldine |
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| DE19850645C1 (en) * | 1998-11-04 | 2000-03-23 | Ruetgers Vft Ag | Single stage recovery of high purity isoquinoline, useful e.g. as starting material for drugs or dyes, by crystallizing isoquinoline fraction from coal-tar having restricted quinoline and quinaldine contents |
| CN1396156A (en) * | 2001-07-13 | 2003-02-12 | 朱景力 | Process for effectively purifying isoquinoline |
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