CN100537507C - Method and apparatus for purifying vitamin A intermediate mynistic aldehyde - Google Patents
Method and apparatus for purifying vitamin A intermediate mynistic aldehyde Download PDFInfo
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- CN100537507C CN100537507C CNB2007100091161A CN200710009116A CN100537507C CN 100537507 C CN100537507 C CN 100537507C CN B2007100091161 A CNB2007100091161 A CN B2007100091161A CN 200710009116 A CN200710009116 A CN 200710009116A CN 100537507 C CN100537507 C CN 100537507C
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Abstract
This invention relates to purification method of intermedium myristic aldehyde and device. The device has set heater, fractionating tower, falling film reboiler, falling film evaporator and condenser. Raw myristic aldehyde outlet of heater connect with fractionating tower inlet; steam outlet of fractionating tower top connect with condenser steam inlet; one way of first condenser condensed fluid outlet connect with reflux liquid inlet of fractionating tower top, the other way outflow low boiler of beta - ionone. Dephlegmation tower bottom outlet respectively connect with falling film reboiler overhead entrance and falling film evaporator overhead entrance; falling film reboiler bottom outlet connect with fractionating tower bottom entrance; one way of falling film evaporator outlet connect with second condenser entrance, the other way is outlet of high boil thing; second condenser outlet is outlet of refine myristic aldehyde. Whil purification first send raw myristic aldehyde to fractionating tower, gain distillate from fractionating tower top. The distillate enter fractionating tower bottom tower kettle, pass through falling film evaporator to remove high boil thing.
Description
Technical field
The present invention relates to a kind of vitamin A intermediate, especially relate to a kind of method of purification of vitamin A intermediate tetradecyl aldehyde.
Background technology
β-14 carbon aldehyde (abbreviation tetradecyl aldehyde) is the important intermediate of synthesise vitamins A, and its structural formula is as follows:
Tetradecyl aldehyde is made through condensation reaction by β-jononeionone usually, and the thick tetradecyl aldehyde that makes of reaction generally contains 80%～86% tetradecyl aldehyde, β-jononeionone of 4%～8%, 8%～12% high boiling material and other material of 1%～2%.
Jononeionone is the reactant of preparation tetradecyl aldehyde, its physicochemical property and tetradecyl aldehyde have certain similarity, a kind of production method of β-jononeionone is provided in the application for a patent for invention of publication number for CN1348949, under the strong acid effect, carry out ring-closure reaction by citrylideneacetone, citrylideneacetone is with after monochloro methane mixes, carry out ring-closure reaction in vitriol oil effect, water or diluted acid water dilution then, termination reaction.Through oil, aqueous phase separation, water is carried the dense one-tenth vitriol oil and is applied mechanically, and oil phase gets β-jononeionone finished product through decompression and solvent recovery after the continuous rectification.Publication number is that disclosing a kind of in the application for a patent for invention of CN1434016 is the method that spices is produced in the rectifying of raw material heat scission reaction with the violet alcohol ester.This method thermal-arrest scission reaction-rectifying separation is in one, and raw material at the cut of the overhead collection of installing to different boiling ranges, obtains the target product of different purity through reactive distillation, identifies that through mass spectrum and chromatogram purity is the poly-beans trienes spices more than 95%.
Traditional tetradecyl aldehyde process for purification is to adopt batch distillation.The problem that this method exists is: (1) batch distillation is a kind of erratic process, tetradecyl aldehyde can not be separated fully with β-jononeionone, and the tetradecyl aldehyde purity that polishing obtains is not high, generally has only 90%～94%; (2) tetradecyl aldehyde material high-temperature heating time in still kettle long, produce unnecessary reducing side reaction, thereby refining yield is not high.
Summary of the invention
The objective of the invention is the problem that exists in the existing tetradecyl aldehyde process for purification, the method for purification of the higher vitamin A intermediate tetradecyl aldehyde of a kind of yield and purity is provided.
Another object of the present invention provides a kind of purifying plant of vitamin A intermediate tetradecyl aldehyde.
Technical scheme of the present invention is to separate unreacted β-jononeionone, remove high boiling material through falling-film evaporator again by continuous rectification, thereby improves refining yield of tetradecyl aldehyde and purity method.
The purifying plant of vitamin A intermediate tetradecyl aldehyde of the present invention is provided with well heater, rectifying tower, falling liquid film reboiler, falling-film evaporator and condenser, the thick tetradecyl aldehyde outlet of well heater connects the rectifying tower inlet, rectifying tower top vapour outlet connects the steam-in of first condenser, a road of the condensed fluid outlet of first condenser connects the top phegma inlet of rectifying tower, and the low-boiling-point substance of β-jononeionone is flowed out on another road.The bottom still material outlet of rectifying tower connects the top still material inlet of falling liquid film reboiler and the top still material inlet of falling-film evaporator respectively, the outlet at bottom of falling liquid film reboiler connects the bottom inlet of rectifying tower, the outlet one tunnel of falling-film evaporator connects the inlet of second condenser, another road is the high boiling material outlet, and the outlet of second condenser is refining tetradecyl aldehyde outlet.
The method of purification of vitamin A intermediate tetradecyl aldehyde of the present invention may further comprise the steps:
1) the thick tetradecyl aldehyde that will contain β-jononeionone is sent into rectifying tower, and the rectifying tower decompression operation gets overhead product from the rectifying tower top, and overhead product is that main component is the low-boiling-point substance of β-jononeionone;
2) main component is that the low-boiling-point substance of β-jononeionone enters rectifier bottoms tower still, and tower still material obtains refining tetradecyl aldehyde after falling-film evaporator removes high boiling material.
After the thick tetradecyl aldehyde that will contain β-jononeionone is sent into rectifying tower, the heat of rectifying tower is provided by rectifying Tata still reboiler, rectifying tower is preferably under the absolute pressure that is lower than 3mmHg and operates, get back to the volume of material of rectifying tower and the reflux ratio of the low-boiling-point substance that receives after regulating condensation, reflux ratio is preferably 3～6.Rectifying Tata still reboiler can adopt the falling film type reboiler.
Compare with the method for purification of existing vitamin A intermediate tetradecyl aldehyde, outstanding advantage of the present invention is:
(1) because rectifying tower adopts high-performance fillers (for example screen waviness packings) and successive rectifying, therefore can stablize and obtain containing the refining tetradecyl aldehyde of tetradecyl aldehyde more than 98%, improve product purity, and then improve the quality and the yield of end product vitamin A;
(2) low-boiling-point substance that steams of rectifying tower top reclaims unreacted β-jononeionone and can utilize again after purification processes, has reduced β-jononeionone reaction unit consumption, thereby has reduced production costs;
(3) because material adds thermal recovery falling liquid film reboiler and falling-film evaporator, adopt falling-film evaporator to remove high boiling material, heated time is short, therefore reduces tetradecyl aldehyde and reduces side reaction, and improves the yield of tetradecyl aldehyde purifying technique.
Description of drawings
Fig. 1 is the purifying plant and the process flow diagram of vitamin A intermediate tetradecyl aldehyde of the present invention.
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
As shown in Figure 1, the purifying plant of vitamin A intermediate tetradecyl aldehyde of the present invention is provided with well heater 1, rectifying tower 2, falling liquid film reboiler 3, falling-film evaporator 4, first condenser 5 and second condenser 6.Thick tetradecyl aldehyde A enters from the inlet of well heater 1, the thick tetradecyl aldehyde outlet of well heater 1 connects the inlet of rectifying tower 2, the overhead vapor outlet of rectifying tower 2 connects the steam-in of first condenser 5, a road of the condensed fluid outlet of first condenser 5 connects the top phegma inlet of rectifying tower 2, and the low-boiling-point substance B of β-jononeionone is flowed out on another road.The bottom still material outlet of rectifying tower 2 connects the top still material inlet of falling liquid film reboiler 3 and the top still material inlet of falling-film evaporator 4 respectively, the outlet at bottom of falling liquid film reboiler 3 connects the bottom inlet of rectifying tower 2, the outlet one tunnel of falling-film evaporator 4 connects the inlet of second condenser 6, another road is the high boiling material outlet, high boiling material C flows out from the high boiling material outlet, the outlet of second condenser 6 is flowed out refining tetradecyl aldehyde D for refining tetradecyl aldehyde outlet, refining tetradecyl aldehyde outlet.
The thick tetradecyl aldehyde heater via of sloughing behind the reaction solvent is heated near entering rectifying tower 2 behind the bubble point temperature.Rectifying tower 2 adopts efficiently, little screen waviness packings falls in pressure.Rectifying tower decompression operation (referring to table 1), the steam that rectifying tower 2 tops steam is condensed into liquid through first condenser 5, a phlegma part is returned rectifying tower 2 as phegma, and another part receives the low-boiling-point substance that obtains main component β-jononeionone, and reflux ratio is 3～6.Tower still material after the discharging of tower still feed liquid, by falling-film evaporator 4, obtains high boiling material by the reception of falling-film evaporator 4 bottoms through 3 heating of falling liquid film reboiler, and steam is condensed into liquid through second condenser 6, receives to obtain refining tetradecyl aldehyde.
The diameter of rectifying tower 2 can adopt 300mm, interior dress screen waviness packings, its composition is as shown in table 2, thick tetradecyl aldehyde is heated to 100 ℃ with the flow heater via 1 of 100kg/h, enter rectifying tower 2, the operational condition of rectifying tower 2 is as shown in table 2, the rectifying tower top reflux ratio is 3～4, the rectifying tower top overhead product is for containing the low-boiling-point substance of 74.8% (calculating by mass percentage) β-jononeionone, and tower still material enters falling-film evaporator 4, at vacuum tightness 3mmHg, under 150～155 ℃ of the interior temperature of falling-film evaporator, evaporative condenser obtains refining tetradecyl aldehyde, and flow is 82.4kg/h, forms to see Table 3.
Table 1 rectifying tower operational condition
The thick tetradecyl aldehyde of table 2 is formed
The refining tetradecyl aldehyde of table 3 is formed
Claims (5)
1. the purifying plant of vitamin A intermediate tetradecyl aldehyde, it is characterized in that being provided with well heater, rectifying tower, the falling liquid film reboiler, falling-film evaporator and condenser, the thick tetradecyl aldehyde outlet of well heater connects the rectifying tower inlet, rectifying tower top vapour outlet connects the steam-in of first condenser, a road of the condensed fluid outlet of first condenser connects the top phegma inlet of rectifying tower, the low-boiling-point substance of β-jononeionone is flowed out on another road, the bottom still material outlet of rectifying tower connects the top still material inlet of falling liquid film reboiler and the top still material inlet of falling-film evaporator respectively, the outlet at bottom of falling liquid film reboiler connects the bottom inlet of rectifying tower, the outlet one tunnel of falling-film evaporator connects the inlet of second condenser, another road is the high boiling material outlet, and the outlet of second condenser is refining tetradecyl aldehyde outlet.
2. the method for purification of vitamin A intermediate tetradecyl aldehyde is characterized in that may further comprise the steps:
1) the thick tetradecyl aldehyde that will contain β-jononeionone is sent into rectifying tower, and the rectifying tower decompression operation gets overhead product from the rectifying tower top, and overhead product is that main component is the low-boiling-point substance of β-jononeionone;
2) main component is that the low-boiling-point substance of β-jononeionone enters rectifier bottoms tower still, and tower still material obtains refining tetradecyl aldehyde after falling-film evaporator removes high boiling material.
3. the method for purification of vitamin A intermediate tetradecyl aldehyde as claimed in claim 2 is characterized in that after the thick tetradecyl aldehyde that will contain β-jononeionone is sent into rectifying tower the heat of rectifying tower is provided by rectifying Tata still reboiler.
4. the method for purification of vitamin A intermediate tetradecyl aldehyde as claimed in claim 2, it is characterized in that described rectifying tower decompression operation operates being lower than under the absolute pressure of 3mmHg, the reflux ratio of regulating volume of material of getting back to rectifying tower after the condensation and the low-boiling-point substance that receives is 3～6.
5. the method for purification of vitamin A intermediate tetradecyl aldehyde as claimed in claim 3 is characterized in that rectifying Tata still reboiler is selected from the falling film type reboiler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100091161A CN100537507C (en) | 2007-06-18 | 2007-06-18 | Method and apparatus for purifying vitamin A intermediate mynistic aldehyde |
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| CNB2007100091161A CN100537507C (en) | 2007-06-18 | 2007-06-18 | Method and apparatus for purifying vitamin A intermediate mynistic aldehyde |
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| CN101070277A CN101070277A (en) | 2007-11-14 |
| CN100537507C true CN100537507C (en) | 2009-09-09 |
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| CN101961562B (en) * | 2010-10-19 | 2012-09-26 | 常州吉恩化工有限公司 | Rectification device |
| CN102091432B (en) * | 2010-12-23 | 2013-01-09 | 厦门金达威集团股份有限公司 | 3-methyl-2-penten-4-yn-1-ol vitamin A intermediate purifying method and device |
| CN102503915B (en) * | 2011-10-25 | 2013-11-20 | 靖江泰达香料化工有限公司 | Peach aldehyde continuous reaction device |
| CN102391216B (en) * | 2011-10-25 | 2013-08-07 | 靖江泰达香料化工有限公司 | Peach aldehyde rectification equipment |
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| CN102531984B (en) * | 2011-12-29 | 2013-12-04 | 上虞新和成生物化工有限公司 | Continuous extracting and purifying method of vitamin A intermediate |
| CN102600631B (en) * | 2012-03-28 | 2014-03-12 | 安徽华业香料股份有限公司 | Device and method for purifying delta-decalactone by vacuum batch distillation |
| CN103408411B (en) * | 2013-07-31 | 2015-09-23 | 安徽智新生化有限公司 | A kind of Preparation device for myristyl alcdehyde |
| CN103936642B (en) * | 2014-04-25 | 2016-08-24 | 上虞新和成生物化工有限公司 | The method of purification of vitamin A isomer in a kind of vitamin A mother solution |
| CN104341283A (en) * | 2014-11-10 | 2015-02-11 | 华玉叶 | Purification technology of tetradecanal |
| CN104892381B (en) * | 2015-04-29 | 2016-09-14 | 上虞新和成生物化工有限公司 | A kind of recoverying and utilizing method of C14 aldehyde rectification low boiling by-product |
| CN108440346A (en) * | 2018-05-07 | 2018-08-24 | 浙江嘉化新材料有限公司 | O-toluenesulfonyl chloride method of purification |
| CN108939591A (en) * | 2018-09-29 | 2018-12-07 | 天津中福环保科技股份有限公司 | Heavy solvent recyclable device, its skid structure and heavy solvent recovery method in a kind of dangerous waste process field |
| CN108939593A (en) * | 2018-09-30 | 2018-12-07 | 天津中福环保科技股份有限公司 | High-solidification point high viscosity solvent recyclable device, its skid structure and method in a kind of dangerous waste process field |
| CN115350493A (en) * | 2022-09-15 | 2022-11-18 | 江苏海莱康生物科技有限公司 | Method for separating and purifying eicosapentaenoic acid ethyl ester in fish oil and rectifying device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001122818A (en) * | 2000-09-22 | 2001-05-08 | T Hasegawa Co Ltd | Method for producing 4-(6,6-dimethyl-2- methylenecyclohexyl)-2-methyl-2-butenal |
| CN1348947A (en) * | 2000-10-18 | 2002-05-15 | 浙江新和成股份有限公司 | Prepn process of vitamin A intermediate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001122818A (en) * | 2000-09-22 | 2001-05-08 | T Hasegawa Co Ltd | Method for producing 4-(6,6-dimethyl-2- methylenecyclohexyl)-2-methyl-2-butenal |
| CN1348947A (en) * | 2000-10-18 | 2002-05-15 | 浙江新和成股份有限公司 | Prepn process of vitamin A intermediate |
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Address after: No. 35, Xinchang Road, Xinyang Industrial Area, Haicang investment zone, Fujian, Xiamen Patentee after: Xiamen Kingdomway Group Co. Address before: No. 35, Xinchang Road, Xinyang Industrial Area, Haicang investment zone, Fujian, Xiamen Patentee before: Xiamen Kingdomway Vitamin Corp. |
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Effective date of registration: 20160620 Address after: 361022 35 Xinchang Road, Xinyang Industrial Area, Haicang investment zone, Xiamen, Fujian Patentee after: XIAMEN KINGDOMWAY VITAMIN Co.,Ltd. Patentee after: Xiamen Kingdomway Group Co. Address before: 361022 35 Xinchang Road, Xinyang Industrial Area, Haicang investment zone, Xiamen, Fujian Patentee before: Xiamen Kingdomway Group Co. |
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