CN1250083A - Vanillin extracting and purifying technology - Google Patents
Vanillin extracting and purifying technology Download PDFInfo
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- CN1250083A CN1250083A CN 98120333 CN98120333A CN1250083A CN 1250083 A CN1250083 A CN 1250083A CN 98120333 CN98120333 CN 98120333 CN 98120333 A CN98120333 A CN 98120333A CN 1250083 A CN1250083 A CN 1250083A
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Abstract
One kind of alkali water solution is used to back-extract vanillin from benzene extracting solution and the extracted vanillin is further processed. The process can replace traditional purifying vacuum distillation process and results in higher yield, less power consumption and low cost.
Description
The present invention relates to a kind of vanillin food grade,1000.000000ine mesh new method for extracting, belong to the aroma material preparation technical field.
Vanillin food grade,1000.000000ine mesh new method for extracting of the present invention is to make strippant with alkaline aqueous solution, vanillin food grade,1000.000000ine mesh back extraction from the benzene extraction solution is taken out, and further process and make vanillin food grade,1000.000000ine mesh, to substitute the distillation method preparation technology that tradition is used.Thereby reduced energy consumption, improved yield, reduced product cost.
Vanillin food grade,1000.000000ine mesh is the synthetic perfume of output maximum in the world, is one of most important flavouring agent.Vanillin food grade,1000.000000ine mesh is except that being applied to industries such as foodstuffs industry such as candy, beverage, drinks, and also wide model is applied in makeup, perfumed soap and the tobacco industry, also as chemical reaction intermediate, brightening agent and biochemical reagents.In addition, it still is a kind of active drug that is used for the treatment of epilepsy.So vanillin food grade,1000.000000ine mesh is a kind of fine chemical product with high economic worth.
The natural origin of vanillin food grade,1000.000000ine mesh is an Orchid section plant, as vanilla bean.Industrial products are mainly obtained by chemical synthesis.Synthesis method commonly used has two kinds, and the one, what adopted in the U.S., Canada and West Europe is the xylogen method of raw material with the forestry waste material; Another kind is the nitroso process that China selects for use.No matter adopt the sort of method, resulting all is the vanillin food grade,1000.000000ine mesh raw material, is not pure vanillin food grade,1000.000000ine mesh, need further purify.
The vanillin food grade,1000.000000ine mesh purifying technique that present domestic factory adopts is benzene extraction back distillation, and ethyl alcohol recrystallization is used in the toluene crystallization at last, and its typical process is as follows:
The reaction condensation → benzene extraction → washing → distillation take off benzene → steam towards the steaming →
Vacuum distilling → toluene crystallization → secondary vacuum distillation → ethyl alcohol recrystallization.The shortcoming of this technology is:
1. yield is low, and full-range total recovery is 70%, wherein with twice vacuum distilling loss maximum (＞20%).
2. energy consumption is big.
3. process complexity, facility investment is big.
Carried out many-sided research for addressing these problems many scholars, proposed many extraction process processes, as amino acid system, stable hydrocarbon method or the like is not because a variety of causes all has and can be used widely industrial.
The objective of the invention is to study a kind of new method of purification and substitute traditional distillation method, promptly make strippant with alkaline aqueous solution, vanillin food grade,1000.000000ine mesh back extraction from the benzene extraction solution is taken out, transfer pH to make its crystallization with acid again, send down step processing again and make vanillin food grade,1000.000000ine mesh, to substitute the distillation method of enrichment preparation technology that tradition is used.
Contain three functional groups in the vanillin food grade,1000.000000ine mesh molecule: hydroxyl, methoxyl group and aldehyde radical, its IUPAC called after 4-hydroxyl, 3-methoxybenzaldehyde.Its structure is shown in Figure of description.
Contain hydroxyl in the vanillin food grade,1000.000000ine mesh molecule, make it in the aqueous solution, show slightly acidic (pK=10.14), therefore it can generate salt soluble in water with the alkali effect, the salt that generates in reaction process constantly is dissolved in water, utilize this character vanillin food grade,1000.000000ine mesh can be stripped into water from organic phase, regulate the pH value then, the vanillin food grade,1000.000000ine mesh crystallization is separated out, further send down the step to handle again with isoelectric point method.
Adopt extracting method of the present invention, identical with former technology before the extraction of its benzene with the later technology of toluene crystallization.Its new technological flow is as follows:
Reaction condensation → benzene extraction → washing → alkaline water reextraction → isoelectric point crystallizing
→ filtration → toluene crystallization → ethyl alcohol recrystallization.
The used alkaline aqueous solution of the present invention is the inorganic salt solution of sodium hydroxide or potassium hydroxide, salt of wormwood etc., and its concentration is 0.01-5.0M.
Specific operation process is as follows: the sodium carbonate solution of 1. preparing 1mol/L.2. with this solution the benzene extraction after washing being carried out the secondary countercurrent reextraction gets.3. with 12.5N sulfuric acid anti-stripping agent is transferred and made its crystallization about pH to 5.4. descend the step to handle crystallization.
Adopt technology of the present invention, can improve yield, reduce energy consumption, reduce product cost.
Embodiments of the invention:
Embodiment 1: alkaline aqueous solution reextraction vanillic aldehyde effect table 1 alkaline aqueous solution reextraction vanillic aldehyde effect project NaOH NaOH NaOH Na2CO3 Na2CO3 Na2CO3 concentration of lye MOL/L 4.18 0.2214 0.0931 2.59 0.5 0.05 balance organic phase concentration g/L 27.0 39.2 50.48 1.4 9.1 54.6 distribution coefficients (=Cw/Co) 1.95 1.02 0.57 55.57 7.71 0.45 as can be seen from Table 1, and the extraction successful of sodium carbonate is better than the NaOH with concentration. Therefore selecting yellow soda ash is ideal as strippant.
Embodiment 2: after the isoelectric point crystallizing yield is stripped, transfer the method for iso-electric point to make the vanillin food grade,1000.000000ine mesh crystallization with acid, crystallization yield and add acid and measure relation is arranged has carried out experimental study to this.Test is to contain the benzole soln 25ml of vanillin food grade,1000.000000ine mesh 0.0792g/l, strip with 0.5M Na2CO3 solution 25ml, regulate pH value with 12.5N H2SO4 again and separate out vanillin food grade,1000.000000ine mesh, the results are shown in Table 2: table 2 vanillin food grade,1000.000000ine mesh coarse-grain yield adds acid amount (milliliter) 0.6 1.0 1.1 1.3 1.5, and to separate out back extraction that the calculating of product (gram) 0.9327 1.2804 1.3988 1.3807 1.3912 yield % 53.2 73.1 79.9 78.8 79.4 yields calculates with α=7.71 to the vanillin food grade,1000.000000ine mesh of water be 100%.
Institute's column data is the primary crystallization yield in the table 2, has reached former state of the art, and through multiplexing recovery, yield can reach more than 85%.
Embodiment 3: the macrocrystalline gas chromatographic detection that the new purifying technique of novel process macrocrystalline component analysis obtains the results are shown in Table 3.Table 3 novel process coarse-grain product quality analysis (crude product before the toluene crystallization)
Vanillin food grade,1000.000000ine mesh % low-boiling-point substance % high boiling material % novel process product 99.648 0.335 0.016
See that from table 3 analytical results novel process coarse-grain quality product meets processing requirement.
Claims (3)
1. the novel method extracted of a vanillin food grade,1000.000000ine mesh, it is characterized in that this novel method be with a kind of alkaline aqueous solution with vanillin food grade,1000.000000ine mesh back extraction taking-up from the benzene extraction solution, and further process and make vanillin food grade,1000.000000ine mesh.
2. according to claim 1, it is characterized in that this anti-stripping agent is added acid to be transferred iso-electric point and get the vanillin food grade,1000.000000ine mesh coarse-grain.
3. according to claim 1, it is characterized in that this alkaline aqueous solution comprises: the aqueous solution of inorganic salt such as sodium hydroxide, yellow soda ash, salt of wormwood comprises and uses one or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98120333 CN1084724C (en) | 1998-10-07 | 1998-10-07 | Vanillin extracting and purifying technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98120333 CN1084724C (en) | 1998-10-07 | 1998-10-07 | Vanillin extracting and purifying technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250083A true CN1250083A (en) | 2000-04-12 |
| CN1084724C CN1084724C (en) | 2002-05-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98120333 Expired - Fee Related CN1084724C (en) | 1998-10-07 | 1998-10-07 | Vanillin extracting and purifying technology |
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| CN (1) | CN1084724C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838188A (en) * | 2010-05-07 | 2010-09-22 | 中国人民解放军第三军医大学 | Refining method of methyl or ethyl vanillin |
| WO2013087795A1 (en) * | 2011-12-15 | 2013-06-20 | Rhodia Operations | Method for purifying vanillin by liquid-liquid extraction |
| CN103709021A (en) * | 2013-05-29 | 2014-04-09 | 浙江普洛康裕生物制药有限公司 | Vanillin extraction method |
-
1998
- 1998-10-07 CN CN 98120333 patent/CN1084724C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838188A (en) * | 2010-05-07 | 2010-09-22 | 中国人民解放军第三军医大学 | Refining method of methyl or ethyl vanillin |
| CN101838188B (en) * | 2010-05-07 | 2013-06-05 | 中国人民解放军第三军医大学 | Refining method of methyl or ethyl vanillin |
| WO2013087795A1 (en) * | 2011-12-15 | 2013-06-20 | Rhodia Operations | Method for purifying vanillin by liquid-liquid extraction |
| FR2984314A1 (en) * | 2011-12-15 | 2013-06-21 | Rhodia Operations | PROCESS FOR PURIFYING VANILLIN BY LIQUID-LIQUID EXTRACTION |
| CN103987686A (en) * | 2011-12-15 | 2014-08-13 | 罗地亚运作公司 | Method for purifying vanillin by liquid-liquid extraction |
| JP2015507615A (en) * | 2011-12-15 | 2015-03-12 | ローディア オペレーションズ | Purification of vanillin by liquid-liquid extraction |
| US9126917B2 (en) | 2011-12-15 | 2015-09-08 | Rhodia Operations | Method for purifying vanillin by liquid-liquid extraction |
| CN103709021A (en) * | 2013-05-29 | 2014-04-09 | 浙江普洛康裕生物制药有限公司 | Vanillin extraction method |
| CN103709021B (en) * | 2013-05-29 | 2015-05-13 | 浙江普洛康裕生物制药有限公司 | Vanillin extraction method |
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| Publication number | Publication date |
|---|---|
| CN1084724C (en) | 2002-05-15 |
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