CN1837172B - Use of separating agent used in preparation of vitamin K3 - Google Patents
Use of separating agent used in preparation of vitamin K3 Download PDFInfo
- Publication number
- CN1837172B CN1837172B CN200610046054A CN200610046054A CN1837172B CN 1837172 B CN1837172 B CN 1837172B CN 200610046054 A CN200610046054 A CN 200610046054A CN 200610046054 A CN200610046054 A CN 200610046054A CN 1837172 B CN1837172 B CN 1837172B
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- CN
- China
- Prior art keywords
- separating agent
- naphthoquinones
- organic solvent
- methyl isophthalic
- isophthalic 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.)
- Expired - Fee Related
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Abstract
Tne invention discloses a release agent application of preparing vitamin K3 with extraction method, which comprises the following steps: (1) adding 2-methyl-1, 4-naphthoquinones, organic solvent and accelerant in autoclave; heating-up to 40-60deg.c; (2) keeping the temperature for 1-2 hours; filtering; (3) non-moving and stratifying after filtering to separate organic facies. The invention can improve the product quality and yield.
Description
Technical field
The application of separating agent when the present invention relates to extraction process and preparing the fodder additives vitamin K3.
Background technology
At the intermediates 2-methyl isophthalic acid with the organic solvent extraction vitamin K3, during the 4-naphthoquinones, organic phase and water emulsification are serious, if do not add separating agent, will make two to be separated and to be difficult to carry out, and disengaging time is infinitely prolonged.Cause single devices to yield poorly, yield is low.
Summary of the invention
For improving the deficiencies in the prior art, promptly at the intermediates 2-methyl isophthalic acid with the organic solvent extraction vitamin K3, during the 4-naphthoquinones, organic phase and water emulsification are serious; At this problem, the invention provides a kind of separating agent, add this separating agent at intermediates 2-methyl isophthalic acid with the organic solvent extraction vitamin K3, during the 4-naphthoquinones, make organic phase and water sharp separation, and can improve the quality of products and yield.
The application of separating agent during the preparation vitamin K3, the present invention adopts organic solvent, 2-methyl isophthalic acid, and the 4-naphthoquinones is a main raw material, and selecting tensio-active agent for use is separating agent, extracts under 40～60 ℃ of conditions;
Its detailed process is as follows:
(1) with the 2-methyl isophthalic acid, 4-naphthoquinones, organic solvent, separating agent are quantitatively put in the reactor, are warming up to 40～60 ℃; The adding weight of organic solvent is the 2-methyl isophthalic acid, 5～10 times of 4-naphthoquinones crude product weight; It is the 2-methyl isophthalic acid that separating agent adds weight, 0.05%～0.15% of 4-naphthoquinones crude product weight;
(2) under this temperature condition, kept 1～2 hour, filter;
(3) after filtration finished, static layering was told organic phase.
Organic solvent is trichloromethane, tetracol phenixin, benzene, toluene or dimethylbenzene.
The composition of separating agent is a tensio-active agent.
Described tensio-active agent is one or more among S-60, T-80, NP-10, the NP-15.
Advantage of the present invention is: at the intermediates 2-methyl isophthalic acid with the organic solvent extraction vitamin K3, during the 4-naphthoquinones, organic phase and water emulsive problem have been solved, add separating agent at intermediates 2-methyl isophthalic acid with the organic solvent extraction vitamin K3, during the 4-naphthoquinones, make organic phase and water sharp separation, and can improve the quality of products and yield.
Embodiment
Embodiment 1:
With 132 kilograms of wet 2-methyl isophthalic acids, 4-naphthoquinones, 560 liters of tetracol phenixin, 150 milliliters of catalyzer (S-60) are put into 1M
3In the reactor, stir and heat up, extraction is 1.0 hours under 50 ℃ of conditions, static separation.140 liters of the burnt sodium water solutions that adding has prepared in isolated organic solvent, the proportioning of burnt sodium water solution is: burnt sodium: water=1: 2.Reaction is 3 hours under 50 ℃ of conditions, static separation, and the aqueous solution branch of K3 is gone in the frozen ethanol solution at the ethanolic soln of 0 ℃ of freezing K3 in the left and right sides, keeps 2 hours.Oven dry is gone in centrifugation, solid K 3, and after the oven dry, getting content is 98.12%K
396 kilograms.
Embodiment 2:
With 135 kilograms of wet 2-methyl isophthalic acids, 4-naphthoquinones, 560 liters of dimethylbenzene, 120 milliliters of catalyzer (S-60 and T-80 each 50%) are put into 1M
3In the reactor, stir and heat up, extraction is 1.0 hours under 50 ℃ of conditions, static separation.140 liters of the burnt sodium water solutions that adding has prepared in isolated organic solvent, the proportioning of burnt sodium water solution is: burnt sodium: water=1: 2.Reaction is 3 hours under 50 ℃ of conditions, static separation, and the aqueous solution branch of K3 is gone in the frozen ethanol solution at the ethanolic soln of 0 ℃ of freezing K3 in the left and right sides, keeps 2 hours.Oven dry is gone in centrifugation, solid K 3, and after the oven dry, getting content is 99.98%K
395.5 kilogram.
Embodiment 3:
With 130 kilograms of wet 2-methyl isophthalic acids, 4-naphthoquinones, 560 liters of dimethylbenzene, 120 milliliters of catalyzer (each 40 milliliters of S-60, T-80, OP-15) are put into 1M
3In the reactor, stir and heat up, extraction is 1.0 hours under 50 ℃ of conditions, static separation.140 liters of the burnt sodium water solutions that adding has prepared in isolated organic solvent, the proportioning of burnt sodium water solution is: burnt sodium: water=1: 2.Reaction is 3 hours under 50 ℃ of conditions, static separation, and the aqueous solution branch of K3 is gone in the frozen ethanol solution at the ethanolic soln of 0 ℃ of freezing K3 in the left and right sides, keeps 2 hours.Oven dry is gone in centrifugation, solid K 3, and after the oven dry, getting content is 98.24%K
396.5 kilogram.
Claims (3)
1. the application of separating agent when preparing vitamin K3 is characterized in that: adopt organic solvent, 2-methyl isophthalic acid, 4-naphthoquinones crude product is a main raw material, and selecting tensio-active agent for use is separating agent, extracts under 40～60 ℃ of conditions;
Its detailed process is as follows:
(1) with the 2-methyl isophthalic acid, 4-naphthoquinones crude product, organic solvent, separating agent are quantitatively put in the reactor, are warming up to 40～60 ℃; The adding weight of organic solvent is the 2-methyl isophthalic acid, 5～10 times of 4-naphthoquinones crude product weight; It is the 2-methyl isophthalic acid that separating agent adds weight, 0.05%～0.15% of 4-naphthoquinones crude product weight;
(2) under this temperature condition, kept 1～2 hour, filter;
(3) after filtration finished, static layering was told organic phase.
2. the application of separating agent during preparation vitamin K3 according to claim 1, it is characterized in that: organic solvent is trichloromethane, tetracol phenixin, benzene, toluene or dimethylbenzene.
3. the application of separating agent during preparation vitamin K3 according to claim 2, it is characterized in that: described tensio-active agent is one or more among S-60, T-80, NP-10, the NP-15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610046054A CN1837172B (en) | 2006-03-16 | 2006-03-16 | Use of separating agent used in preparation of vitamin K3 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610046054A CN1837172B (en) | 2006-03-16 | 2006-03-16 | Use of separating agent used in preparation of vitamin K3 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1837172A CN1837172A (en) | 2006-09-27 |
| CN1837172B true CN1837172B (en) | 2010-05-12 |
Family
ID=37014704
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610046054A Expired - Fee Related CN1837172B (en) | 2006-03-16 | 2006-03-16 | Use of separating agent used in preparation of vitamin K3 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1837172B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085266A (en) * | 1992-10-07 | 1994-04-13 | 冶金工业部鞍山热能研究所 | Vitamin K 3Production method and electrolyzer |
| US5329026A (en) * | 1989-11-28 | 1994-07-12 | Nippon Shokubai Kagaku Kogyo Co., Ltd. | Process for preparation of 2-substituted 1,4-naphthoquinone |
-
2006
- 2006-03-16 CN CN200610046054A patent/CN1837172B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5329026A (en) * | 1989-11-28 | 1994-07-12 | Nippon Shokubai Kagaku Kogyo Co., Ltd. | Process for preparation of 2-substituted 1,4-naphthoquinone |
| CN1085266A (en) * | 1992-10-07 | 1994-04-13 | 冶金工业部鞍山热能研究所 | Vitamin K 3Production method and electrolyzer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1837172A (en) | 2006-09-27 |
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Granted publication date: 20100512 Termination date: 20110316 |