CN1326919A - Method for separating and purifying niacin - Google Patents
Method for separating and purifying niacin Download PDFInfo
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- CN1326919A CN1326919A CN 00109066 CN00109066A CN1326919A CN 1326919 A CN1326919 A CN 1326919A CN 00109066 CN00109066 CN 00109066 CN 00109066 A CN00109066 A CN 00109066A CN 1326919 A CN1326919 A CN 1326919A
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- dicarboxylic acid
- acid
- propane
- ethane
- hexanodioic
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Abstract
By using the nylon acid waste liquid produced during the nitric acid oxidation of cyclodexanol and cyclohexanone as main material and water as solvent, and through the repeated crystallization and separation, 1,2-ethanedicarboxylic anhydride and 1,3-propyldicarboxylic acid are extracted. The process has short process, low material consumption, low power consumption and low cost and the present invention can solve the environmental pollution caused by waste.
Description
The present invention relates to a kind of method of separating purifying niacin, relate to specifically in a kind of nylon acid waste liquid that from hexalin and pimelinketone nitric acid oxidation production process, produces, extract and reclaim 1,2-ethane dicarboxylic anhydride and 1, the method for 3-propane dicarboxylic acid.
At present, in the product of industrial chemicals: 1, the purposes of 2-ethane dicarboxylic anhydride is very extensive, but costs an arm and a leg, and market is seriously in short supply; 1, the purposes of 3-propane dicarboxylic acid is more extensive, but still belongs to blank at home.Above-mentioned two kinds of raw materials are domestic rare, and the industrial chemicals of extensive prospect is arranged again.In fact can obtain 1,2-ethane dicarboxylic anhydride and 1,3-propane dicarboxylic acid by separating purification hexalin and pimelinketone nitric acid oxidation waste liquid.Yet domestic recovery and utilization for hexalin and pimelinketone nitric acid oxidation waste liquid just are limited to make and mix binary carboxylic fat (softening agent).In addition, many methods were arranged once also at home and abroad, and as adopting urea complexation, solvent extration, distillation method etc. hexalin and pimelinketone nitric acid oxidation waste liquid were recycled, though the product purity that adopts these methods to reclaim is higher, the rate of recovery is very low; Though some method rate of recovery is higher, the quality product that reclaims is bad.Also have, patent publication No. is the Chinese patent of CN1067046A, because it is to adopt a series of method such as evaporation, fatization, rectifying, hydrolysis to extract dicarboxylic acid and lipid thereof, thus the long flow path of this patent extracting method, the material consumption height, yield is low, its poor effect.
The object of the present invention is to provide a kind ofly from the nitric acid oxidation waste liquid of hexalin and pimelinketone, extract to reclaim 1,2-ethane dicarboxylic anhydride and 1, a kind of method of separating purifying niacin of 3-propane dicarboxylic acid is to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this, it is a major ingredient by the nylon acid waste liquid that produces in hexalin and the pimelinketone nitric acid oxidation production process, with water is solvent, by crystallization, separation, recrystallize, separation again, be that recrystallization extracts 1,2-ethane dicarboxylic anhydride and 1, the method for 3-propane dicarboxylic acid is characterized in that:
1. will be by the nylon acid waste liquid that produces in hexalin and the pimelinketone nitric acid oxidation production process, the water solvent dissolving of weight such as add, in the time of 45 ℃～55 ℃, at first separate out hexanodioic acid and 1, the crystal of 2-ethane dicarboxylic acid, to deliver to distillation tower vacuum distilling behind the dissolution of crystals, 1,2-ethane dicarboxylic anhydride is distilled from cat head and draws, hexanodioic acid goes out from tower bottom flow
2. above-mentioned mother liquor is the recrystallization output crystal second time in the time of 20 ℃～30 ℃, as the mixed dicarboxylic acid raw material
3. its mother liquor cools off in the time of 10 ℃～20 ℃, 1,3-propane dicarboxylic acid crystals is separated out, add that water will separate out 1, the dissolving of 3-propane dicarboxylic acid crystals, recrystallization in the time of 20 ℃～30 ℃ separates it, obtains 1,3-propane dicarboxylic acid product,
4. 2. above-mentioned and mother liquor 3. reclaims vanadium, copper spent catalyst and 1 respectively, the 3-propane dicarboxylic acid aqueous solution through ion exchange resin vanadium removal and copper.
Its feature also is: the vacuum distilling in the distillation tower is in 100mm mercury column vacuum tightness, greater than what carry out under 260 ℃ the condition.
Its feature also is: the relative of nitric acid oxidation gained the by-product mix dicarboxylic acid of hexalin and pimelinketone consists of 1,2-ethane dicarboxylic acid 10-25%, 1, and 3-propane dicarboxylic acid 35-55%, hexanodioic acid 25-45%, its concentration is about 85-95%.
Its feature also is: described 1,2-ethane dicarboxylic acid and hexanodioic acid are to contain 1, be extracted out in the 3-propane dicarboxyl aqueous acid, 1,2-ethane dicarboxylic acid is with 1, the form of 2-ethane dicarboxylic anhydride is separated from the top of distillation tower, hexanodioic acid is to flow out from the tower still, 1, and 3-propane dicarboxylic acid is from having told 1, in the mother liquor of 2-ethane dicarboxylic acid and hexanodioic acid, adopt the method for recrystallization to branch away.
Its feature also is: 1, and the crystallization treatment process of 2-ethane dicarboxylic acid and hexanodioic acid is divided into two stages, and the fs is 40-55 ℃, and subordinate phase is 15-30 ℃; 1, the crystallization treatment process of 3-propane dicarboxylic acid also is divided into two stages, and the fs is 5-20 ℃, and subordinate phase is 15-30 ℃.
Its feature also is: 1, and the crystallization treatment process fs optimum temps of 2-ethane dicarboxylic acid and hexanodioic acid is 45 ℃, the subordinate phase optimum temps is 20 ℃; 1, the crystallization treatment process fs optimum temps of 3-propane dicarboxylic acid is 10 ℃, and the subordinate phase optimum temps is 20 ℃.
The present invention compared with prior art, it is to be solvent with water, adopt the recrystallization method domestic rare industrial chemicals of purifying from waste liquid, and flow process is lacked, energy consumption, material consumption are low, can reduce cost this method technology maturation greatly, easy and simple to handle, less investment has considerable economic and social benefit.Solved simultaneously the waste pollution problem of environment again.
Further specify the present invention below in conjunction with drawings and Examples
Accompanying drawing is a schema of the present invention.
Embodiment
1. will be by nylon acid waste liquid 100 grams that produce in hexalin and the pimelinketone nitric acid oxidation production process, the water solvent that adds 100 grams, send among the dissolving crystallized jar of I and dissolve, crystallisation by cooling in the time of 45 ℃, separate out hexanodioic acid and 1, the crystal of 2-ethane dicarboxylic acid is isolated hexanodioic acid and 1 through separator 1, the crystal I47 gram of 2-ethane dicarboxylic acid, the crystal I of 47 grams are delivered among the dissolving vessel I and dissolve, send into distillation tower after the dissolving, in 100mm mercury column vacuum tightness, greater than vacuum distilling under 260 ℃ the condition, go out 1 of 21 grams from the cat head fractionation by distillation, 2-ethane dicarboxylic anhydride goes out 26 hexanodioic acids that restrain from tower bottom flow
2. the mother liquor of telling among the separator I is sent among the crystallizer H, the recrystallization output crystal second time in the time of 20 ℃, and deliver among the separator II, hexanodioic acid and 1,2-ethane dicarboxylic acid crystals is separated again, gets hexanodioic acid and 1, the crystal II20 gram of 2-ethane dicarboxylic acid recrystallization, and place dissolving vessel II as the mixed dicarboxylic acid raw material, deliver to after the dissolving among the dissolving crystallized jar of I
3. the mother liquor of telling among the separator II is sent among the crystallizer III, cooling in the time of 10 ℃, 1,3-propane dicarboxylic acid crystals is separated out, and is sent among the separator III and separates, and gets 1, the crystal III of 3-propane dicarboxylic acid, deliver among the dissolving crystallized jar of IV, water is with crystal III dissolving, recrystallization in the time of 20 ℃ again, deliver among the separator IV and separate, obtain 1 of 38 grams, the recrystallization crystal of 3-propane dicarboxylic acid is a product
4. the mother liquor among the separator III is sent to catalyst recovery devices together together with the mother liquor among the separator IV, through ion exchange resin vanadium removal and copper, reclaim vanadium, copper spent catalyst and 1 respectively, the 3-propane dicarboxylic acid aqueous solution, 1, the 3-propane dicarboxylic acid aqueous solution can be used as the dissolving water of raw material.
Claims (6)
1, a kind of method of separating purifying niacin, it is a major ingredient by the nylon acid waste liquid that produces in hexalin and the pimelinketone nitric acid oxidation production process, with water is solvent, by crystallization, separation, recrystallize, separation again, be that recrystallization method extracts 1,2-ethane dicarboxylic anhydride and 1, the method for 3-propane dicarboxylic acid is characterized in that:
1. will be by the nylon acid waste liquid that produces in hexalin and the pimelinketone nitric acid oxidation production process, the water solvent dissolving of weight such as add, in the time of 45 ℃～55 ℃, at first separate out hexanodioic acid and 1, the crystal of 2-ethane dicarboxylic acid, to deliver to distillation tower vacuum distilling behind the dissolution of crystals, 1,2-ethane dicarboxylic anhydride is distilled from cat head and draws, hexanodioic acid goes out from tower bottom flow
2. above-mentioned mother liquor is the recrystallization output crystal second time in the time of 20 ℃～30 ℃, as the mixed dicarboxylic acid raw material
3. its mother liquor cools off in the time of 10 ℃～20 ℃, 1,3-propane dicarboxylic acid crystals is separated out, add that water will separate out 1, the dissolving of 3-propane dicarboxylic acid crystals, recrystallization in the time of 20 ℃～30 ℃ separates it, obtains 1,3-propane dicarboxylic acid product,
4. 2. above-mentioned and mother liquor 3. reclaims vanadium, copper spent catalyst and 1 respectively, the 3-propane dicarboxylic acid aqueous solution through ion exchange resin vanadium removal and copper.
2, a kind of method of separating purifying niacin according to claim 1, its feature also is: the vacuum distilling in the distillation tower is in 100mm mercury column vacuum tightness, greater than what carry out under 260 ℃ the condition.
3, a kind of method of separating purifying niacin according to claim 1, its feature also is: the relative of nitric acid oxidation gained the by-product mix dicarboxylic acid of hexalin and pimelinketone consists of 1,2-ethane dicarboxylic acid 10-25%, 1,3-propane dicarboxylic acid 35-55%, hexanodioic acid 25-45%, its concentration is about 85-95%.
4, a kind of method of separating purifying niacin according to claim 1, its feature also is: described 1,2-ethane dicarboxylic acid and hexanodioic acid are to contain 1, are extracted out in the 3-propane dicarboxyl aqueous acid, 1,2-ethane dicarboxylic acid is with 1, and the form of 2-ethane dicarboxylic anhydride is separated from the top of distillation tower, and hexanodioic acid is to flow out from the tower still, 1,3-propane dicarboxylic acid is from having told 1, in the mother liquor of 2-ethane dicarboxylic acid and hexanodioic acid, having adopted the method for recrystallization to branch away.
5, a kind of method of separating purifying niacin according to claim 1, its feature also is: 1, the crystallization treatment process of 2-ethane dicarboxylic acid and hexanodioic acid is divided into two stages, and the fs is 40-55 ℃, and subordinate phase is 15-30 ℃; 1, the crystallization treatment process of 3-propane dicarboxylic acid also is divided into two stages, and the fs is 5-20 ℃, and subordinate phase is 15-30 ℃.
6, a kind of method of separating purifying niacin according to claim 1, its feature also is: 1, the crystallization treatment process fs optimum temps of 2-ethane dicarboxylic acid and hexanodioic acid is 45 ℃, the subordinate phase optimum temps is 20 ℃; 1, the crystallization treatment process fs optimum temps of 3-propane dicarboxylic acid is 10 ℃, and the subordinate phase optimum temps is 20 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00109066 CN1326919A (en) | 2000-06-05 | 2000-06-05 | Method for separating and purifying niacin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00109066 CN1326919A (en) | 2000-06-05 | 2000-06-05 | Method for separating and purifying niacin |
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| CN1326919A true CN1326919A (en) | 2001-12-19 |
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| CN 00109066 Pending CN1326919A (en) | 2000-06-05 | 2000-06-05 | Method for separating and purifying niacin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003013A (en) * | 2017-06-23 | 2018-05-08 | 河南城建学院 | A kind of recoverying and utilizing method of nylon acid |
| CN109734578A (en) * | 2019-01-14 | 2019-05-10 | 重庆华峰化工有限公司 | The method of purification and product and purposes of a kind of adipic acid by-product mixed dibasic acid |
-
2000
- 2000-06-05 CN CN 00109066 patent/CN1326919A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003013A (en) * | 2017-06-23 | 2018-05-08 | 河南城建学院 | A kind of recoverying and utilizing method of nylon acid |
| CN109734578A (en) * | 2019-01-14 | 2019-05-10 | 重庆华峰化工有限公司 | The method of purification and product and purposes of a kind of adipic acid by-product mixed dibasic acid |
| CN109734578B (en) * | 2019-01-14 | 2022-05-20 | 重庆华峰化工有限公司 | Purification method of adipic acid by-product mixed dibasic acid, product and application |
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