CN114409523A - Preparation method of 1, 3-acetonedicarboxylic acid - Google Patents
Preparation method of 1, 3-acetonedicarboxylic acid Download PDFInfo
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- CN114409523A CN114409523A CN202111647274.6A CN202111647274A CN114409523A CN 114409523 A CN114409523 A CN 114409523A CN 202111647274 A CN202111647274 A CN 202111647274A CN 114409523 A CN114409523 A CN 114409523A
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- acid
- acetonedicarboxylic
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- concentrated sulfuric
- temperature
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- OXTNCQMOKLOUAM-UHFFFAOYSA-N 3-Oxoglutaric acid Chemical compound OC(=O)CC(=O)CC(O)=O OXTNCQMOKLOUAM-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 59
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000012043 crude product Substances 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 8
- 238000004537 pulping Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000010009 beating Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229960004106 citric acid Drugs 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 2
- WTQYWNWRJNXDEG-UHFFFAOYSA-N 6-Hydroxy-hyoscyamin Natural products CN1C(C2)CC(O)C1CC2OC(=O)C(CO)C1=CC=CC=C1 WTQYWNWRJNXDEG-UHFFFAOYSA-N 0.000 description 1
- 229930003347 Atropine Natural products 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- RKUNBYITZUJHSG-UHFFFAOYSA-N Hyosciamin-hydrochlorid Natural products CN1C(C2)CCC1CC2OC(=O)C(CO)C1=CC=CC=C1 RKUNBYITZUJHSG-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229960004543 anhydrous citric acid Drugs 0.000 description 1
- WTQYWNWRJNXDEG-LEOABGAYSA-N anisodamine Chemical compound C1([C@@H](CO)C(=O)O[C@@H]2C[C@H]3[C@@H](O)C[C@@H](C2)N3C)=CC=CC=C1 WTQYWNWRJNXDEG-LEOABGAYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- RKUNBYITZUJHSG-SPUOUPEWSA-N atropine Chemical compound O([C@H]1C[C@H]2CC[C@@H](C1)N2C)C(=O)C(CO)C1=CC=CC=C1 RKUNBYITZUJHSG-SPUOUPEWSA-N 0.000 description 1
- 229960000396 atropine Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- -1 sulfuric acid compound Chemical class 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method of 1, 3-acetone dicarboxylic acid. The preparation method comprises the following steps: reacting concentrated sulfuric acid with citric acid to obtain feed liquid containing 1, 3-acetone dicarboxylic acid; cooling the obtained feed liquid to below 10 ℃, adding water at 0-5 ℃, cooling to 5-10 ℃ after the addition is finished, and carrying out solid-liquid separation to obtain a crude product of the 1, 3-acetonedicarboxylic acid; mixing the 1, 3-acetonedicarboxylic acid crude product with ethyl acetate, pulping, carrying out solid-liquid separation, and drying to obtain the 1, 3-acetonedicarboxylic acid. The preparation method provided by the invention can be used for preparing the 1, 3-acetonedicarboxylic acid product with higher quality and yield.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of 1, 3-acetone dicarboxylic acid.
Background
1, 3-acetonedicarboxylic acid (Dimethyl acetate-1, 3-dicarboxylate or 3-oxo-pentanedioic acid) is colorless needle-like crystals, has a melting point of 135 deg.C (decomposed), is readily soluble in water and alcohol, and is insoluble in chloroform and benzene. 1, 3-acetone dicarboxylic acid is an aliphatic chain molecule, is a medical intermediate, and is applied to the synthesis of atropine and anisodamine in the twentieth century. Since the century, it was found that it has a certain antibacterial activity, it has been widely used in the synthesis of antibiotic drugs.
The conventional method is to oxidize anhydrous citric acid by sulfuryl chloride or fuming sulfuric acid to produce acetone dicarboxylic acid and acetone dicarboxylic ester, wherein the content of the acetone dicarboxylic acid is difficult to exceed 97.5 percent, and the fuming sulfuric acid has high requirements on equipment and poor production safety and is not beneficial to industrial production. The production of 1, 3-acetonedicarboxylic acid using concentrated sulfuric acid instead of oleum has also been reported. However, the existing process for producing 1, 3-acetonedicarboxylic acid has the defects of more side reactions, low product yield and poor quality, and needs to be further improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of 1, 3-acetonedicarboxylic acid. The method can prepare the 1, 3-acetone dicarboxylic acid product with higher quality and yield.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of 1, 3-acetone dicarboxylic acid, which comprises the following steps:
(1) reacting concentrated sulfuric acid with citric acid to obtain feed liquid containing 1, 3-acetone dicarboxylic acid;
(2) cooling the feed liquid obtained in the step (1) to below 10 ℃, adding water at 0-5 ℃, cooling to 5-10 ℃ after the addition is finished, and carrying out solid-liquid separation to obtain a crude product of the 1, 3-acetonedicarboxylic acid;
(3) mixing the 1, 3-acetonedicarboxylic acid crude product with ethyl acetate, pulping, carrying out solid-liquid separation, and drying to obtain the 1, 3-acetonedicarboxylic acid.
In some embodiments of the invention, the concentrated sulfuric acid has a concentration of 98 wt% or more.
In some embodiments of the invention, the mass ratio of sulfuric acid to citric acid in step (1) is 6-7: 1; for example, 6:1, 6.2:1, 6.3:1, 6.5:1, 6.6:1, 6.8:1, or 7:1, etc. may be used. The mass ratio is a ratio of the mass of the sulfuric acid compound contained in the concentrated sulfuric acid to the mass of the citric acid.
In some embodiments of the present invention, the citric acid is added to the concentrated sulfuric acid in a batch manner in the step (1) to perform the reaction.
In some embodiments of the present invention, during the adding of the citric acid, the temperature of the mixed solution of concentrated sulfuric acid and citric acid is controlled below 35 ℃; for example, it may be 35 ℃, 34 ℃, 32 ℃, 30 ℃, 28 ℃, 25 ℃, 22 ℃, 20 ℃, 18 ℃, 15 ℃, 12 ℃, 10 ℃ or 5 ℃.
In some embodiments of the invention, the temperature of the reaction in step (1) is 35-40 ℃; for example, it may be 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃ or 40 ℃.
In some embodiments of the invention, the reaction time in step (1) is 5 to 8 hours; for example, it may be 5h, 5.5h, 6h, 6.5h, 7h, 7.5h, 8h, or the like.
In some embodiments of the invention, the mass ratio of the water added in step (2) to the concentrated sulfuric acid is 0.6-0.7: 1; for example, it may be 0.6:1, 0.62:1, 0.63:1, 0.65:1, 0.66:1, 0.68:1, or 0.7: 1.
In some embodiments of the present invention, during the adding of the water in the step (2), the temperature of the mixed solution of the feed liquid and the water is controlled below 20 ℃; for example, the temperature may be 18 ℃, 16 ℃, 15 ℃, 13 ℃, 12 ℃, 10 ℃ or 8 ℃.
In some embodiments of the invention, the mass ratio of ethyl acetate to crude 1, 3-acetonedicarboxylic acid in step (3) is 1: 1.5-1.6; for example, 1:1.5, 1:1.52, 1:1.53, 1:1.55, 1:1.56, 1:1.58, or 1:1.6, etc. may be mentioned.
In some embodiments of the invention, the temperature of the mixing and beating in the step (3) is 0-5 ℃; for example, it may be 0 ℃, 1 ℃, 2 ℃,3 ℃, 4 ℃ or 5 ℃.
In some embodiments of the invention, the drying in step (3) is vacuum drying below 40 ℃.
In some embodiments of the invention, the preparation method comprises the following steps:
(1) adding concentrated sulfuric acid into a reactor, cooling to 0-5 ℃ under the stirring condition, adding citric acid into the concentrated sulfuric acid in batches after the cooling is finished, controlling the temperature of a mixed solution of the concentrated sulfuric acid and the citric acid to be below 35 ℃ in the adding process, and carrying out heat preservation reaction at 35-40 ℃ for 5-8h after the adding is finished to obtain a feed liquid containing 1, 3-acetonedicarboxylic acid;
(2) cooling the feed liquid obtained in the step (1) to below 10 ℃, adding water at 0-5 ℃, controlling the temperature of the mixed liquid of the feed liquid and the water to be below 20 ℃ in the adding process, cooling to 5-10 ℃ after the adding is finished, and performing centrifugal separation to obtain a crude product of the 1, 3-acetonedicarboxylic acid;
(3) mixing the 1, 3-acetonedicarboxylic acid crude product and ethyl acetate at 0-5 ℃, pulping, centrifugally separating, and drying in vacuum at the temperature of below 40 ℃ to obtain the 1, 3-acetonedicarboxylic acid.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method provided by the invention optimizes the process conditions such as process temperature, material proportion, purification solvent and the like, so that the purity of the obtained 1, 3-acetonedicarboxylic acid product reaches more than 98%, and the yield reaches more than 88%.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the specific embodiments are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
This example provides a method for preparing 1, 3-acetonedicarboxylic acid, comprising the steps of:
(1) cleaning and drying a 1500L reactor to ensure that reaction equipment is anhydrous;
adding 1000kg of 98% concentrated sulfuric acid into a reactor, starting stirring, cooling to 3 ℃, adding 150kg of citric acid into the reactor in batches after cooling is finished, and finishing feeding for 5 hours until the temperature of materials in the reactor is 33 ℃;
after the feeding is finished, heating to 36 ℃, and carrying out heat preservation reaction for 8 hours to obtain feed liquid containing 1, 3-acetonedicarboxylic acid;
(2) cooling the feed liquid obtained in the step (1) to 10 ℃, slowly adding 600kg of water at 0 ℃, controlling the temperature of the mixed liquid of the feed liquid and the water to be below 20 ℃ in the adding process, adding water for 4 hours, then cooling to 10 ℃, discharging and carrying out centrifugal separation to obtain 120kg of crude 1, 3-acetonedicarboxylic acid;
(3) adding the crude 1, 3-acetonedicarboxylic acid into 77kg of ethyl acetate, cooling to 5 ℃, fully pulping, performing centrifugal separation, and performing vacuum drying at 30 ℃ to obtain 102.2kg of refined 1, 3-acetonedicarboxylic acid.
Example 2
This example provides a method for preparing 1, 3-acetonedicarboxylic acid, comprising the steps of:
(1) cleaning and drying a 1500L reactor to ensure that reaction equipment is anhydrous;
adding 1000kg of 98% concentrated sulfuric acid into a reactor, starting stirring, cooling to 3 ℃, adding 150kg of citric acid into the reactor in batches after cooling is finished, and finishing feeding for 5 hours until the temperature of materials in the reactor is 33 ℃;
after the feeding is finished, heating to 40 ℃, and carrying out heat preservation reaction for 5 hours to obtain feed liquid containing 1, 3-acetonedicarboxylic acid;
(2) cooling the feed liquid obtained in the step (1) to 5 ℃, slowly adding 700kg of water at 5 ℃, controlling the temperature of the mixed liquid of the feed liquid and the water to be below 20 ℃ in the adding process, adding water for 4 hours, then cooling to 5 ℃, discharging and carrying out centrifugal separation to obtain 123kg of crude 1, 3-acetonedicarboxylic acid;
(3) adding the crude 1, 3-acetonedicarboxylic acid into 77kg of ethyl acetate, cooling to 0 ℃, fully pulping, performing centrifugal separation, and performing vacuum drying at 30 ℃ to obtain 101.9kg of refined 1, 3-acetonedicarboxylic acid.
Example 3
This example provides a method for preparing 1, 3-acetonedicarboxylic acid, comprising the steps of:
(1) cleaning and drying a 1500L reactor to ensure that reaction equipment is anhydrous;
adding 1000kg of 98% concentrated sulfuric acid into a reactor, starting stirring, cooling to 3 ℃, adding 150kg of citric acid into the reactor in batches after cooling is finished, and finishing feeding for 5 hours until the temperature of materials in the reactor is 33 ℃;
after the feeding is finished, heating to 38 ℃, and carrying out heat preservation reaction for 6 hours to obtain feed liquid containing 1, 3-acetonedicarboxylic acid;
(2) cooling the feed liquid obtained in the step (1) to 3 ℃, slowly adding 650kg of water at 3 ℃, controlling the temperature of the mixed liquid of the feed liquid and the water to be below 20 ℃ in the adding process, adding water for 4 hours, then cooling to 7 ℃, discharging and carrying out centrifugal separation to obtain 122.5kg of crude 1, 3-acetonedicarboxylic acid;
(3) adding the crude 1, 3-acetonedicarboxylic acid into 77kg of ethyl acetate, cooling to 3 ℃, fully pulping, performing centrifugal separation, and performing vacuum drying at 30 ℃ to obtain 102.1kg of refined 1, 3-acetonedicarboxylic acid.
Example 4
This example provides a process for the preparation of 1, 3-acetonedicarboxylic acid, differing from example 1 only in that the reaction temperature in step (1) is 45 ℃.
Example 5
This example provides a process for producing 1, 3-acetonedicarboxylic acid, differing from example 1 only in that the mass of concentrated sulfuric acid in step (1) is 600kg, and the amount of water added in step (2) is 360kg (the mass ratio of concentrated sulfuric acid to water is the same as in example 1).
Comparative example 1
A process for producing 1, 3-acetonedicarboxylic acid, which is different from example 1 only in that the temperature of water added in step (2) is 23 ℃, is provided.
Comparative example 2
Provided is a method for producing 1, 3-acetonedicarboxylic acid, which is different from example 1 only in that the amount of water added in step (2) is 500 kg.
Comparative example 3
There is provided a process for producing 1, 3-acetonedicarboxylic acid, which is different from example 1 only in that ethyl acetate in step (3) is replaced with methanol.
The purity of the 1, 3-acetonedicarboxylic acid refined products obtained in the above examples and comparative examples was measured by liquid chromatography, and the yield was calculated, with the results shown in table 1 below:
TABLE 1
| Sample (I) | Purity (%) | Yield (%) |
| Example 1 | 98.6 | 88.2 |
| Example 2 | 98.5 | 88.0 |
| Example 3 | 98.3 | 88.1 |
| Example 4 | 85.3 | 75.1 |
| Example 5 | 83.6 | 73.3 |
| Comparative example 1 | 66.8 | 52.3 |
| Comparative example 2 | 85.1 | 86.5 |
| Comparative example 3 | 79.1 | 73.2 |
As can be seen from Table 1, the purity of the 1, 3-acetonedicarboxylic acid prepared by the method provided by the invention reaches more than 83%, and the yield reaches more than 73%. By optimizing the process conditions, the purity of the 1, 3-acetone dicarboxylic acid reaches more than 98 percent, and the yield reaches more than 88 percent.
Among them, in example 4, the reaction temperature was higher than that in example 1, and thus side reactions were more likely to occur, and the purity and yield of the obtained 1, 3-acetonedicarboxylic acid were lowered. In example 5, the reaction was insufficient due to a small amount of concentrated sulfuric acid, and the purity and yield of the obtained 1, 3-acetonedicarboxylic acid were lowered.
Compared with example 1, the use of normal temperature water in step (2) of comparative example 1 results in difficulty in controlling the temperature of the feed during the addition process, and more side reactions occur when the temperature reaches above 50 ℃, so that the purity and yield of the obtained 1, 3-acetonedicarboxylic acid are significantly reduced. Comparative example 2 the amount of water added was small, resulting in a product with a high level of inclusion impurities and a relatively low purity of the 1, 3-acetonedicarboxylic acid. In comparative example 3, methanol was used instead of ethyl acetate, and the purification effect was deteriorated, and thus the purity and yield of 1, 3-acetonedicarboxylic acid obtained were remarkably decreased.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of 1, 3-acetone dicarboxylic acid is characterized by comprising the following steps:
(1) reacting concentrated sulfuric acid with citric acid to obtain feed liquid containing 1, 3-acetone dicarboxylic acid;
(2) cooling the feed liquid obtained in the step (1) to below 10 ℃, adding water at 0-5 ℃, cooling to 5-10 ℃ after the addition is finished, and carrying out solid-liquid separation to obtain a crude product of the 1, 3-acetonedicarboxylic acid;
(3) mixing the crude 1, 3-acetonedicarboxylic acid product with ethyl acetate, pulping, carrying out solid-liquid separation, and drying to obtain a refined 1, 3-acetonedicarboxylic acid product.
2. The production method according to claim 1, wherein the concentrated sulfuric acid has a concentration of 98 wt% or more.
3. The production method according to claim 1 or 2, wherein the mass ratio of sulfuric acid to citric acid in step (1) is 6-7: 1.
4. The production method according to any one of claims 1 to 3, wherein the citric acid is added to concentrated sulfuric acid in a batch manner in step (1) to perform a reaction;
preferably, the temperature of the mixed solution of concentrated sulfuric acid and citric acid is controlled to be below 35 ℃ during the addition of the citric acid.
5. The method according to any one of claims 1 to 4, wherein the temperature of the reaction in step (1) is 35 to 40 ℃;
preferably, the reaction time in step (1) is 5-8 h.
6. The production method according to any one of claims 1 to 5, wherein the mass ratio of the water added in step (2) to the concentrated sulfuric acid is 0.6 to 0.7: 1.
7. The method according to any one of claims 1 to 6, wherein the temperature of the mixed solution of the feed liquid and water is controlled to 20 ℃ or lower during the addition of the water in the step (2).
8. The production method according to any one of claims 1 to 7, wherein the mass ratio of the ethyl acetate to the crude 1, 3-acetonedicarboxylic acid in the step (3) is 1:1.5 to 1.6;
preferably, the temperature of the mixing and beating in the step (3) is 0-5 ℃.
9. The production method according to any one of claims 1 to 8, wherein the drying in step (3) is vacuum drying at 40 ℃ or lower.
10. The production method according to any one of claims 1 to 9, characterized by comprising the steps of:
(1) adding concentrated sulfuric acid into a reactor, cooling to 0-5 ℃ under the stirring condition, adding citric acid into the concentrated sulfuric acid in batches after the cooling is finished, controlling the temperature of a mixed solution of the concentrated sulfuric acid and the citric acid to be below 35 ℃ in the adding process, and carrying out heat preservation reaction at 35-40 ℃ for 5-8h after the adding is finished to obtain a feed liquid containing 1, 3-acetonedicarboxylic acid;
(2) cooling the feed liquid obtained in the step (1) to below 10 ℃, adding water at 0-5 ℃, controlling the temperature of the mixed liquid of the feed liquid and the water to be below 20 ℃ in the adding process, cooling to 5-10 ℃ after the adding is finished, and performing centrifugal separation to obtain a crude product of the 1, 3-acetonedicarboxylic acid;
(3) mixing the 1, 3-acetonedicarboxylic acid crude product and ethyl acetate at 0-5 ℃, pulping, centrifugally separating, and drying in vacuum at the temperature of below 40 ℃ to obtain the 1, 3-acetonedicarboxylic acid.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101475482A (en) * | 2009-01-22 | 2009-07-08 | 杭州同化化学有限公司 | Preparation of dimethyl acetone-1,3-dicarboxylate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475482A (en) * | 2009-01-22 | 2009-07-08 | 杭州同化化学有限公司 | Preparation of dimethyl acetone-1,3-dicarboxylate |
Non-Patent Citations (2)
| Title |
|---|
| 唐新军;徐建兵;臧阳陵;: "丙酮二羧酸及其衍生物的合成研究", 精细化工中间体 * |
| 马明轩: "雷尼酸锶的合成及制剂工艺分析", 《医药化工》 * |
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