CN102838473A - High-purity acetyl chloride and preparation method thereof - Google Patents
High-purity acetyl chloride and preparation method thereof Download PDFInfo
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- CN102838473A CN102838473A CN 201110182503 CN201110182503A CN102838473A CN 102838473 A CN102838473 A CN 102838473A CN 201110182503 CN201110182503 CN 201110182503 CN 201110182503 A CN201110182503 A CN 201110182503A CN 102838473 A CN102838473 A CN 102838473A
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- acetyl chloride
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- phosphorus trichloride
- chloride 98min
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Abstract
The invention relates to an acetyl chloride, and in particular relates to a high-purity acetyl chloride and a preparation method thereof, belonging to the field of chemical technologies. In the method, acetic acid and phosphorus trichloride are adopted, the reaction temperature is controlled to be 25-30 DEG C, and high-purity acetyl chloride can be obtained by reaction and technologies such as rectification. The preparation method has the advantages that a catalyst is adopted in the reaction process, the reaction temperature is lowered, side reactions are reduced, the yield is greatly improved, and the yield of crude product is increased to more than 97% from 91% after reaction. The light distillate which is less in amount and mainly comprises acetyl chloride and hydrogen chloride generated during rectification can be basically absorbed by rectification residual liquid reaction, and can take part in the reaction in a circulating way, so that the emission of waste liquid and the absorption of alkaline liquor are reduced, the side reactions can be reduced, the operation environment is improved, and the reaction yield is indirectly improved.
Description
Technical field
The present invention relates to a kind of Acetyl Chloride 98Min., be specifically related to a kind of high-purity Acetyl Chloride 98Min. and preparation method thereof, belong to chemical technology field.
Background technology
Acetyl Chloride 98Min. is a kind of important organic synthesis intermediate and acetylation reagent, and acidylate ability force rate acetic anhydride is strong, is widely used in organic synthesis.Can be used for producing agricultural chemicals, medicine, novel complexant for electroplating, and other multiple Minute Organic Synthesis midbody, pharmaceutically can be used for making 2.4 1 dichlor fluorbenzenes (midbody of CIPROFLOXACIN USP 24), Ibuprofen BP/EP etc.Acetyl Chloride 98Min. also is the catalyzer of carboxylic acid generation chlorination reaction, also can be used for hydroxyl and amino quantitative analysis.Traditional acetic acid and phosphorus trichloride synthesis method; Utilize the sub product (being the bullion Acetyl Chloride 98Min.) of producing acetic anhydride type linking agent to make with extra care and get; The principal feature of this method be production technique simple (only needing rectifying) but its quality product is relatively low, can not satisfy the high standard requirement.
Summary of the invention
The objective of the invention is for overcoming the weak point of above-mentioned prior art; A kind of high-purity Acetyl Chloride 98Min. and preparation method thereof is provided; This method adopts acetic acid and phosphorus trichloride, and temperature of reaction is controlled to be 25 ℃-30 ℃, promptly obtains high-purity Acetyl Chloride 98Min. through technologies such as reaction and rectifying and produces.
The present invention realizes with following technical scheme: a kind of high-purity Acetyl Chloride 98Min. is characterized in that: comprise acetic acid and catalyzer, described catalyzer is a phosphorus trichloride; The mole proportioning of acetic acid and phosphorus trichloride is 3: 1.20, and temperature of reaction is 25 ℃-30 ℃.
Prepare the method for the described a kind of high-purity Acetyl Chloride 98Min. of claim 1, it is characterized in that: comprise the steps:
Step 1, acetic acid, catalyzer are added in the reactor drum by weight, stir cooling, the phosphorus trichloride of getting ready by proportioning; Slowly in reactor drum, drip phosphorus trichloride then, temperature of reaction is 25 ℃-30 ℃, drip phosphorus trichloride after; Continue stirring reaction, leave standstill layering behind the 0.5h;
Step 2, lower floor are the mixture of sub product phosphorous acid and excessive phosphorus trichloride, can continue rectifying and receive phosphorus trichloride wherein; The upper strata is mainly the Acetyl Chloride 98Min. bullion, and the Acetyl Chloride 98Min. bullion carries out conventional rectification through rectifying tower, and the lighting end in early stage is an Acetyl Chloride 98Min., and the cut of collecting 51-52 ℃ promptly obtains high-purity Acetyl Chloride 98Min. product;
Raffinate after step 3, the rectifying is the suction resorber then, absorbs the Acetyl Chloride 98Min. that captures in the light fraction when treating down to criticize rectifying, and the circulation participation is reacted, utilized again in the Returning reactor again.
Advantage of the present invention is: adopted catalyzer in this preparing method's the reaction process, reduced temperature of reaction, reduced the side reaction generation, improved yield greatly, reacted bullion yield rises to more than 97% by 91%.Can be distillated basically raffinate reaction of the light fraction that produces during rectifying (comparatively small amt mainly contains Acetyl Chloride 98Min., hydrogenchloride etc.) absorbs, and reaction is participated in circulation; Reduced the discharging of waste liquid and absorbed with alkali lye; Reduce side reaction, improved operating environment, also improved reaction yield indirectly.
Embodiment
Embodiment,
A kind of high-purity Acetyl Chloride 98Min. comprises acetic acid and catalyzer, and described catalyzer is a phosphorus trichloride; The mole proportioning of acetic acid and phosphorus trichloride is 3: 1.20, and temperature of reaction is 25 ℃-30 ℃.
Prepare the method for the described a kind of high-purity Acetyl Chloride 98Min. of claim 1, it is characterized in that: comprise the steps:
Step 1, acetic acid, catalyzer are added in the reactor drum by weight, stir cooling, the phosphorus trichloride of getting ready by proportioning; Slowly in reactor drum, drip phosphorus trichloride then, temperature of reaction is 25 ℃-30 ℃, drip phosphorus trichloride after; Continue stirring reaction, leave standstill layering behind the 0.5h;
Step 2, lower floor are the mixture of sub product phosphorous acid and excessive phosphorus trichloride, can continue rectifying and receive phosphorus trichloride wherein; The upper strata is mainly the Acetyl Chloride 98Min. bullion, and the Acetyl Chloride 98Min. bullion carries out conventional rectification through rectifying tower, and the lighting end in early stage is an Acetyl Chloride 98Min., and the cut of collecting 51-52 ℃ promptly obtains high-purity Acetyl Chloride 98Min. product;
Raffinate after step 3, the rectifying is the suction resorber then, absorbs the Acetyl Chloride 98Min. that captures in the light fraction when treating down to criticize rectifying, and the circulation participation is reacted, utilized again in the Returning reactor again.
Claims (2)
1. high-purity Acetyl Chloride 98Min., it is characterized in that: comprise acetic acid and catalyzer, described catalyzer is a phosphorus trichloride; The mole proportioning of acetic acid and phosphorus trichloride is 3: 1.20, and temperature of reaction is 25 ℃-30 ℃.
2. prepare the method for the described a kind of high-purity Acetyl Chloride 98Min. of claim 1, it is characterized in that: comprise the steps:
Step 1, acetic acid, catalyzer are added in the reactor drum by weight, stir cooling, the phosphorus trichloride of getting ready by proportioning; Slowly in reactor drum, drip phosphorus trichloride then, temperature of reaction is 25 ℃-30 ℃, drip phosphorus trichloride after; Continue stirring reaction, leave standstill layering behind the 0.5h;
Step 2, lower floor are the mixture of sub product phosphorous acid and excessive phosphorus trichloride, can continue rectifying and receive phosphorus trichloride wherein; The upper strata is mainly the Acetyl Chloride 98Min. bullion, and the Acetyl Chloride 98Min. bullion carries out conventional rectification through rectifying tower, and the lighting end in early stage is an Acetyl Chloride 98Min., and the cut of collecting 51-52 ℃ promptly obtains high-purity Acetyl Chloride 98Min. product;
Raffinate after step 3, the rectifying is the suction resorber then, absorbs the Acetyl Chloride 98Min. that captures in the light fraction when treating down to criticize rectifying, and the circulation participation is reacted, utilized again in the Returning reactor again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110182503 CN102838473A (en) | 2011-06-24 | 2011-06-24 | High-purity acetyl chloride and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110182503 CN102838473A (en) | 2011-06-24 | 2011-06-24 | High-purity acetyl chloride and preparation method thereof |
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| Publication Number | Publication Date |
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| CN102838473A true CN102838473A (en) | 2012-12-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201110182503 Pending CN102838473A (en) | 2011-06-24 | 2011-06-24 | High-purity acetyl chloride and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019145304A1 (en) * | 2018-01-25 | 2019-08-01 | Akzo Nobel Chemicals International B.V. | Process for the production of a fertilizer |
| CN115073286A (en) * | 2022-07-02 | 2022-09-20 | 山东国邦药业有限公司 | Method for producing acetyl chloride and nitric acid by using tail gas containing nitroxyl chloride |
-
2011
- 2011-06-24 CN CN 201110182503 patent/CN102838473A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019145304A1 (en) * | 2018-01-25 | 2019-08-01 | Akzo Nobel Chemicals International B.V. | Process for the production of a fertilizer |
| CN111655614A (en) * | 2018-01-25 | 2020-09-11 | 诺力昂化学品国际有限公司 | Method for producing fertilizer |
| CN115073286A (en) * | 2022-07-02 | 2022-09-20 | 山东国邦药业有限公司 | Method for producing acetyl chloride and nitric acid by using tail gas containing nitroxyl chloride |
| CN115073286B (en) * | 2022-07-02 | 2024-05-14 | 山东国邦药业有限公司 | Method for producing acetyl chloride and nitric acid by utilizing tail gas containing nitroxyl chloride |
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Application publication date: 20121226 |