CN102190567B - Treatment method for decarboxylation and extraction emulsifying layer in production process of ethyl vanillin - Google Patents
Treatment method for decarboxylation and extraction emulsifying layer in production process of ethyl vanillin Download PDFInfo
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- CN102190567B CN102190567B CN201010123105.8A CN201010123105A CN102190567B CN 102190567 B CN102190567 B CN 102190567B CN 201010123105 A CN201010123105 A CN 201010123105A CN 102190567 B CN102190567 B CN 102190567B
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- Prior art keywords
- emulsion layer
- layer
- decarboxylation
- emulsifying layer
- emulsifying
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- CBOQJANXLMLOSS-UHFFFAOYSA-N ethyl vanillin Chemical compound CCOC1=CC(C=O)=CC=C1O CBOQJANXLMLOSS-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000001804 emulsifying effect Effects 0.000 title claims abstract description 23
- 238000006114 decarboxylation reaction Methods 0.000 title claims abstract description 17
- 229940073505 ethyl vanillin Drugs 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 238000000605 extraction Methods 0.000 title abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000012074 organic phase Substances 0.000 claims abstract description 19
- 238000004062 sedimentation Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 230000005494 condensation Effects 0.000 claims abstract description 4
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 239000000839 emulsion Substances 0.000 claims description 40
- 239000008346 aqueous phase Substances 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 150000001879 copper Chemical class 0.000 abstract 3
- 239000012071 phase Substances 0.000 abstract 2
- 238000006482 condensation reaction Methods 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 235000012970 cakes Nutrition 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000012631 food intake Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a treatment method for a decarboxylation and extraction emulsifying layer in the production process of ethyl vanillin. In the production process of ethyl vanillin, glyoxylate and 2-thanatol as starting materials are subjected to condensation, oxidation and decarboxylation reaction to generate the ethyl vanillin; the decarboxylation and extraction emulsifying layer is an emulsifying layer formed by extracting the ethyl vanillin from a reaction solution by utilizing methylbenzene after the decarboxylation reaction is finished; and in the treatment method of the emulsifying layer, the emulsifying layer is treated by using a sedimentation centrifuge; the vast majority of organic phase and part of insoluble copper salt are separated from the emulsifying layer; and the emulsifying layer subjected to the sedimentation centrifuge treatment is treated by using a tubular-bowl centrifuge, so that residual organic phase and insoluble copper salts in the emulsifying layer are completely separated from the water phase. By using the treatment method, the emulsifying layer is treated by adopting a two-step method of sedimentation centrifuge and tubular-bowl centrifuge, the organic phase, the water phase and the insoluble copper salts in the emulsifying layer can be completely separated; and the treatment method disclosed by the invention has the advantages of simplicity and convenience for operation, quickness, high efficiency, low cost, and the like.
Description
Technical field
The present invention relates to chemical field, particularly the treatment process of decarboxylation extracting and emulsifying layer in production process of ethyl vanillin.
Background technology
Vanirone (chemistry vanirom by name) has the milk of XIANGJIALANDOU fragrance and dense wish, for broad spectrum type spices, its purposes is very extensive, as in food, daily use chemicals, tobacco industry as perfume material, correctives or fixative, wherein the food consumption such as beverage, candy, cake, biscuit, bread and roasted seeds and nuts is in the majority.
At present, the synthesis of vanirone mainly with oxoethanoic acid and 2-thanatol for starting raw material, obtained through condensation, oxidation and decarboxylic reaction.
After decarboxylic reaction terminates, vanirone need be extracted with toluene from reaction solution.But in extraction process, the mix and blend of water and toluene can produce a large amount of emulsion layers.Emulsion layer is present between aqueous phase and organic phase interface, not only containing aqueous phase and organic phase, and containing more insoluble mantoquita.If emulsion layer is integrated with aqueous phase and discharges, aqueous phase COD (chemical oxygen demand (COD)) being caused to exceed standard because of the toluene wherein contained on the one hand, loss of product be caused because of being dissolved with product in toluene on the other hand; If emulsion layer is integrated with organic phase and enters next technique, again can because of water and the bringing into of impurity and affect normally carrying out of subsequent processing of being dissolved in the water.Therefore, the organic phase in emulsion layer, aqueous phase must be separated completely with insoluble mantoquita.
The method of existing process emulsion layer mainly contains filtration method (comprising vacuum filtration, filter press, common centrifuging etc.) and breakdown of emulsion method (comprise salt adding breakdown of emulsion, breakdown of emulsion etc. of heating), but all there is more deficiency.The maximum deficiency of filtration method is that the insoluble mantoquita in emulsion layer can block filter cloth, and cause filter effect low, waste time and energy, also need further stratification after filtration, vacuum filtration also can cause a large amount of losses of solvent.The maximum deficiency of breakdown of emulsion method is then need salt adding or heat, and cause cost increase, impurity increase, and effect is also very limited, can not fundamentally deal with problems.
Summary of the invention
In view of this, the object of the present invention is to provide the treatment process of decarboxylation extracting and emulsifying layer in a kind of production process of ethyl vanillin, can fast and efficiently the organic phase in emulsion layer, aqueous phase be separated completely with insoluble mantoquita three.
For achieving the above object, the present invention adopts following technical scheme:
The treatment process of decarboxylation extracting and emulsifying layer in production process of ethyl vanillin, described production process of ethyl vanillin is with oxoethanoic acid and 2-thanatol for starting raw material, generates vanirone through condensation, oxidation and decarboxylic reaction; The emulsion layer that described decarboxylation extracting and emulsifying layer is formed when being and extracting vanirone with toluene from reaction solution after decarboxylic reaction terminates; The treatment process of described emulsion layer is first by the process of emulsion layer settling centrifuge, most organic phase in emulsion layer and the insoluble mantoquita of part are separated, again by the tubular-bowl centrifuge process of the emulsion layer after sedimentation centrifugal treating, make remaining organic phase in emulsion layer, insoluble mantoquita is separated completely with aqueous phase.
In production process of ethyl vanillin, the main ingredient of decarboxylation extracting and emulsifying layer is organic phase, aqueous phase and insoluble mantoquita.Because the proportion of organic phase is little compared with other composition, the proportion of insoluble mantoquita is large compared with aqueous phase, therefore, first emulsion layer settling centrifuge filters by the present invention, most light composition in emulsion layer and organic phase are separated, the inwall that simultaneously in emulsion layer, the insoluble mantoquita of about 60% can be adsorbed on settling centrifuge is separated; Then by the process of centrifugal for sedimentation rear remaining emulsion layer tubular-bowl centrifuge, from its light fraction outlet separable go out remaining organic phase emulsion layer, from the outlet of its heavy constituent separable go out aqueous phase emulsion layer, and the inwall that in emulsion layer, the insoluble mantoquita of remaining about 40% can be adsorbed on tubular-bowl centrifuge to be separated; Thus, emulsion layer is through two-step pretreatment, and organic phase wherein, aqueous phase are well separated with insoluble mantoquita.
Beneficial effect of the present invention is: the present invention adopts decarboxylation extracting and emulsifying layer in the centrifugal and tubular type centrifugal two-step approach process production process of ethyl vanillin of sedimentation, in emulsion layer, the resolution of organic phase is not less than 99%, the resolution of insoluble mantoquita reaches 100%, both the loss of organic phase institute lysate in emulsion layer had been avoided, the COD that turn avoid discharge of wastewater exceeds standard, also assures that the recovery of insoluble mantoquita simultaneously, there is the advantages such as easy and simple to handle, quick, efficient, with low cost.
Accompanying drawing explanation
In order to make the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the present invention is described in further detail, wherein:
Accompanying drawing is the inventive method schematic diagram.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
The decarboxylation extracting and emulsifying layer of preferred embodiment process is brown, after measured, its contain 42% toluene, the water of 57%, the insoluble mantoquita of 0.6% and 0.4% other component.
The SSC600G type settling centrifuge used in preferred embodiment and GQLY150 rocking type channel separator are produced by Liaoyang sunlight pharmaceutical machine company limited.
As shown in drawings, the treatment process of decarboxylation extracting and emulsifying layer comprises the following steps:
A, sedimentation are centrifugal: to be transferred to by 200L emulsion layer in hold-up vessel (after measured, emulsion layer temperature is 28 DEG C, pH value is 4), open hold-up vessel dispensing valve, emulsion layer adds in settling centrifuge gradually through pipeline, to be fed to whizzer about 2/3 volume time stop liquid feeding, open whizzer, the slash liquid mouth of pipe from whizzer after half a minute has toluene to flow out, and collects the toluene of outflow in toluene tank; When skimming the liquid mouth of pipe and flowing out without toluene, regulate and skim liquid pipe position, continue to collect the toluene flowed out; When slash liquid pipe to be regulated also flows out without toluene, stop toluene collecting, slash liquid pipe is adjusted to distance whizzer wall proximal most position, then the emulsion layer after sedimentation centrifugal treating is collected into water storage tank.Collect completely, slash liquid pipe is adjusted to starting position, continues to add pending emulsion layer, repeat aforesaid operations, until all emulsion layers are disposed, about 30 minutes treatment times.Collection obtains toluene 76L, the emulsion layer 118L after sedimentation centrifugal treating, insoluble mantoquita (being adsorbed on the inwall of settling centrifuge) weight in wet base 4Kg altogether.
B, tubular type are centrifugal: storage tank valve of fetching boiling water, the emulsion layer after sedimentation centrifugal treating allowing step a collect slowly flows into tubular-bowl centrifuge, open whizzer, after 1 minute, toluene is had to flow out from the light fraction outlet of whizzer, heavy constituent outlet simultaneously there are flowing out, and collection toluene and water are to toluene tank and water storage tank respectively, about 30 minutes treatment times.Collection obtains toluene 6L, water 110L, insoluble mantoquita (being adsorbed on the inwall of tubular-bowl centrifuge) weight in wet base 3Kg altogether.
Adopt decarboxylation extracting and emulsifying layer 200L in the centrifugal and tubular type centrifugal two-step approach process production process of ethyl vanillin of sedimentation, total consuming time about 1 hour, toluene separation efficiency is 99%, and insoluble mantoquita separation efficiency is 100%.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (1)
1. the treatment process of decarboxylation extracting and emulsifying layer in production process of ethyl vanillin, described production process of ethyl vanillin be with oxoethanoic acid and 2-thanatol for starting raw material, generate vanirone through condensation, oxidation and decarboxylic reaction; The emulsion layer that described decarboxylation extracting and emulsifying layer is formed when being and extracting vanirone with toluene from reaction solution after decarboxylic reaction terminates; It is characterized in that: the treatment process of described emulsion layer is first by the process of emulsion layer settling centrifuge, most organic phase in emulsion layer and the insoluble mantoquita of part are separated, again by the tubular-bowl centrifuge process of the emulsion layer after sedimentation centrifugal treating, make remaining organic phase in emulsion layer, insoluble mantoquita is separated completely with aqueous phase; Described settling centrifuge is SSC600G type settling centrifuge, and described tubular-bowl centrifuge is GQLY150 rocking type channel separator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010123105.8A CN102190567B (en) | 2010-03-12 | 2010-03-12 | Treatment method for decarboxylation and extraction emulsifying layer in production process of ethyl vanillin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010123105.8A CN102190567B (en) | 2010-03-12 | 2010-03-12 | Treatment method for decarboxylation and extraction emulsifying layer in production process of ethyl vanillin |
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| Publication Number | Publication Date |
|---|---|
| CN102190567A CN102190567A (en) | 2011-09-21 |
| CN102190567B true CN102190567B (en) | 2015-06-17 |
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| CN201010123105.8A Active CN102190567B (en) | 2010-03-12 | 2010-03-12 | Treatment method for decarboxylation and extraction emulsifying layer in production process of ethyl vanillin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4165341A (en) * | 1977-02-04 | 1979-08-21 | Ube Industries, Ltd. | Process for preparing protocatechualdehyde and its derivatives |
| CN1258399C (en) * | 2003-06-07 | 2006-06-07 | 吉化集团公司 | Oxydation catalyst used in synthesizing 4-hydroxy 3-methoxy benzaldehyde and 4-hydroxyl-3-ethoxy benzaldehyde by glyoxalic acid method |
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- 2010-03-12 CN CN201010123105.8A patent/CN102190567B/en active Active
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| Title |
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| 化学工业部人事教育司 化学工业部教育培训中心.离心分离.《液相非均一系分离》.化学工业出版社,1997,(第1版),第253、256-258页. * |
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| CN102190567A (en) | 2011-09-21 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhao Huawen Inventor after: Hong Wei Inventor after: Wei Yong Inventor after: Yang Lijun Inventor after: Liu Xushan Inventor after: Tan Xiuwan Inventor after: Chen Jie Inventor before: Zhao Huawen Inventor before: Hong Wei Inventor before: Wei Yong Inventor before: Yang Lijun Inventor before: Liu Xushan Inventor before: Tan Xiuwan Inventor before: Chen Jie |
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Address after: 401220 No.2, Huanan No.1 Branch Road, Yanjia chemical industry park, Changshou District, Chongqing Patentee after: Chongqing Xinxin Xiangrong Fine Chemical Co.,Ltd. Address before: No. 2 Huanan 1st Road, Chemical Industry Park, Changshou District, Chongqing, 401221 Patentee before: CHONGQING THRIVE CHEMICAL Co.,Ltd. |