CN104072350A - Method for preparing vanillin - Google Patents
Method for preparing vanillin Download PDFInfo
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- CN104072350A CN104072350A CN201410264621.0A CN201410264621A CN104072350A CN 104072350 A CN104072350 A CN 104072350A CN 201410264621 A CN201410264621 A CN 201410264621A CN 104072350 A CN104072350 A CN 104072350A
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- mixture
- food grade
- vanillin
- mesh
- acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/51—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition
- C07C45/511—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition involving transformation of singly bound oxygen functional groups to >C = O groups
- C07C45/512—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition involving transformation of singly bound oxygen functional groups to >C = O groups the singly bound functional group being a free hydroxyl group
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/367—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of functional groups containing oxygen only in singly bound form
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing vanillin and relates to the technical field of chemical engineering. The method comprises the following steps of mixing wood phenols, alkali, glyoxylic acid and sulfuric acid to carry out condensation, carrying out extractive distillation, adding air, water and alkali, carrying out oxidative decarboxylation reaction, adding an acid for acidifying treatment, then adding toluene, concentrating for extracting, distilling the mixture extracted by concentrating to filter the residue off, putting the mixture and methanol into a crystallization vessel and crystallizing, and putting the crystallized mixture into a centrifugal device to separate out methanol mother liquor, drying the mixture subjected to centrifugal separation to obtain a vanillin product, packaging and warehousing. The method disclosed by the invention has the beneficial effects of simpleness and convenience in preparation, less yield of waste acid, less investment in equipment, high purity and convenience in operation and the prepared vanillin has a good application effect and is safe and reliable.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to a kind of preparation method of vanillin food grade,1000.000000ine mesh.
Background technology
Vanillin food grade,1000.000000ine mesh, has another name called Vanillin, for a kind of widely used edible spices, can in the seed of vanilla, find, also can synthetic, there is strong milk breath.Be widely used in the various blending food that need to increase milk breath, as cake, cold drink, chocolate, candy; Also can be used for perfumed soap, toothpaste, perfume, rubber, plastics, pharmaceuticals.Vanillin food grade,1000.000000ine mesh is one of important flavouring agent, it is edible deodorant tune, there is XIANGJIALANDOU fragrance and strong milk, it is indispensable important source material in foodstuff additive industry, be widely used in the various blending food that need to increase milk breath, as played flavouring and fixation effect in cake, cold drink, chocolate, candy, biscuit, instant noodles, bread and tobacco, blending drinks, toothpaste, soap, perfume, makeup, ice-creams, beverage and daily cosmetics.Vanillin food grade,1000.000000ine mesh Application Areas is abroad very wide, in a large number for the production of medicine intermediate, also for plant growth promoter, sterilant, lubricating oil antifoams, brightening agent, printed circuit board, produces conductive agent etc.Domestic vanillin food grade,1000.000000ine mesh is mainly used in foodstuff additive, constantly widens in recent years in the application of field of medicaments, has become vanillin food grade,1000.000000ine mesh and has applied most potential field.Current domestic vanillin food grade,1000.000000ine mesh consumption: foodstuffs industry accounts for 55%, and medicine intermediate accounts for 30%, and feed seasonings accounts for 10%, and makeup etc. account for 5%.Both at home and abroad Industry China is world vanillin food grade,1000.000000ine mesh big export country, and within 2002, domestic needs amount is 2350 tons, accounts for 30% of output, and all the other are 70% for outlet.And 1988 be only outlet 273 tons, within 1993, be 1700 tons, within 2002, be 4653 tons.1993～2002 years, Chinese vanillin food grade,1000.000000ine mesh export volume average growth rate per annum was 12%, and traditional vanillin food grade,1000.000000ine mesh production technique is comparatively complicated, and the purity of producing is lower, is difficult to meet human wants.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of purity high, prepares the preparation method of simple vanillin food grade,1000.000000ine mesh.
Technical problem to be solved by this invention realizes by the following technical solutions:
A preparation method for vanillin food grade,1000.000000ine mesh, is characterized in that: comprise following processing step,
A. by wooden phenol, alkali, oxoethanoic acid, sulfuric acid mixes and carries out condensation.
B. the mixture after condensation in a is carried out to extractive distillation.
C. will in the mixture after extractive distillation in b, add air, water and alkali carry out oxidative decarboxylation reaction.
D. concentrated by adding acid to carry out adding again toluene to extract after acidification in the reacted mixture of oxidative decarboxylation.
E. the mixture after extraction being concentrated distills filtering residue and mixture drops in crystallization kettle.
F. at crystallization kettle, dropping into methyl alcohol carries out mixture to carry out crystallization treatment.
G. the mixture after crystallization is dropped into centrifugal device and isolate methanol mother liquor.
H. the mixture after centrifugation is carried out to drying treatment, obtain vanillin food grade,1000.000000ine mesh finished product packing warehouse-in.
Toluene in described step b after distillation processing adopts withdrawing can to reclaim, and reuses.
In described steps d, extract the toluene recovery after concentrating, and the waste water producing flows into the unified processing of accumulator tank.
The invention has the beneficial effects as follows: the present invention is easy to prepare simple, and spent acid generation is few, and facility investment is few, and purity is high, convenient operation, the vanillin food grade,1000.000000ine mesh result of use of preparation is good, safe and reliable.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
A preparation method for vanillin food grade,1000.000000ine mesh, is characterized in that: comprise following processing step,
A. by wooden phenol, alkali, oxoethanoic acid, sulfuric acid mixes and carries out condensation.
B. the mixture after condensation in a is carried out to extractive distillation, the toluene after distillation is processed adopts withdrawing can to reclaim, and reuses
C. just in the mixture after extractive distillation, add air in b, water and alkali carry out oxidative decarboxylation reaction.
D. concentrated by adding acid to carry out adding again toluene to extract after acidification in the reacted mixture of oxidative decarboxylation, the toluene recovery after extraction is concentrated, and the waste water producing flows into, and accumulator tank is unified to be processed.
E. the mixture after extraction being concentrated distills filtering residue and mixture drops in crystallization kettle.
F. at crystallization kettle, dropping into methyl alcohol carries out mixture to carry out crystallization treatment.
G. the mixture after crystallization is dropped into centrifugal device and isolate methanol mother liquor.
H. the mixture after centrifugation is waken up with a start to drying treatment, obtain vanillin food grade,1000.000000ine mesh finished product packing warehouse-in.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (3)
1. a preparation method for vanillin food grade,1000.000000ine mesh, is characterized in that: comprise following processing step,
A. by wooden phenol, alkali, oxoethanoic acid, sulfuric acid mixes and carries out condensation.
B. the mixture after condensation in a is carried out to extractive distillation.
C. just in the mixture after extractive distillation, add air in b, water and alkali carry out oxidative decarboxylation reaction.
D. concentrated by adding acid to carry out adding again toluene to extract after acidification in the reacted mixture of oxidative decarboxylation.
E. the mixture after extraction being concentrated distills filtering residue and mixture drops in crystallization kettle.
F. at crystallization kettle, dropping into methyl alcohol carries out mixture to carry out crystallization treatment.
G. the mixture after crystallization is dropped into centrifugal device and isolate methanol mother liquor.
H. the mixture after centrifugation is waken up with a start to drying treatment, obtain vanillin food grade,1000.000000ine mesh finished product packing warehouse-in.
2. the preparation method of a kind of vanillin food grade,1000.000000ine mesh according to claim 1, is characterized in that: the toluene in described step b after distillation processing adopts withdrawing can to reclaim.
3. the preparation method of a kind of vanillin food grade,1000.000000ine mesh according to claim 1, is characterized in that: in described steps d, extract the toluene recovery after concentrating, and the waste water producing flows into the unified processing of accumulator tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410264621.0A CN104072350A (en) | 2014-06-13 | 2014-06-13 | Method for preparing vanillin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410264621.0A CN104072350A (en) | 2014-06-13 | 2014-06-13 | Method for preparing vanillin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104072350A true CN104072350A (en) | 2014-10-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410264621.0A Pending CN104072350A (en) | 2014-06-13 | 2014-06-13 | Method for preparing vanillin |
Country Status (1)
| Country | Link |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010310A (en) * | 2010-10-21 | 2011-04-13 | 宁波王龙科技股份有限公司 | Productive technology of vanlillin by glyoxylic acid method |
| CN102276434A (en) * | 2011-06-30 | 2011-12-14 | 辽宁世星药化有限公司 | Method for producing vanillin |
-
2014
- 2014-06-13 CN CN201410264621.0A patent/CN104072350A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010310A (en) * | 2010-10-21 | 2011-04-13 | 宁波王龙科技股份有限公司 | Productive technology of vanlillin by glyoxylic acid method |
| CN102276434A (en) * | 2011-06-30 | 2011-12-14 | 辽宁世星药化有限公司 | Method for producing vanillin |
Non-Patent Citations (2)
| Title |
|---|
| 周亚婷等: "乙醛酸法合成香兰素的研究", 《化工科技》 * |
| 游佳勇等: "乙醛酸制备香兰素工艺条件的优化", 《食品与生物技术学报》 * |
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Application publication date: 20141001 |