CN103739580B - The treatment process of palmitinic acid residue - Google Patents
The treatment process of palmitinic acid residue Download PDFInfo
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- CN103739580B CN103739580B CN201310720183.XA CN201310720183A CN103739580B CN 103739580 B CN103739580 B CN 103739580B CN 201310720183 A CN201310720183 A CN 201310720183A CN 103739580 B CN103739580 B CN 103739580B
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- palmitinic acid
- cetylate
- acid residue
- centrifugal
- ethyl acetate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to chemical technology field, particularly relate to the treatment process of the palmitinic acid residue produced in Quicifal production process, the present invention first carries out rinse removal of impurities with solvent to palmitinic acid residue, then carry out reacting through centrifugal, airing, input xitix successively, purify, crystallization, the operation such as centrifugal, dry, palmitinic acid residue is converted into Quicifal the most at last, and the solvent filtrate wherein obtained in rotary process returns rinse removal of impurities operation.One aspect of the present invention is prepared to tradition the waste residue that Quicifal produces and is processed, avoid it to the pollution of environment, on the other hand the useful matter in waste residue is recycled, become Fei Weibao, during Quicifal is produced, product yield improves more than 10%, and cost reduces by 10% ~ 20%.
Description
Technical field
The present invention relates to chemical technology field, particularly relate to the treatment process of the palmitinic acid residue produced in Quicifal production process.
Background technology
Quicifal (being also VC cetylate) forms for the esterification of the natural component such as palmitinic acid and L-AA, and its molecular formula is C
22h
38o
7, be a kind of oxygen scavenqer and synergistic agent efficiently, be assessed as the foodstuff additive with trophicity, nontoxic, efficient, use safety by the foodstuff additive council of the World Health Organization (WHO).
At present, the preparation method of food antioxidant Quicifal mainly contains chemical process and biological method, wherein chemical process mainly with raw material xitix, palmitinic acid through a series of esterification, purification and obtaining.In order to reach best product yield in production process, palmitinic acid is excessive input, causes producing a large amount of palmitinic acid residue (about 80% ~ 90% be palmitinic acid in residue, 10% ~ 20% be Quicifal and other impurity on a small quantity).All not being used to waste residue in existing explained hereafter not only causes raw material to waste, and causes environmental pollution.
Summary of the invention
In order to solve the problem, the object of the invention is to, a kind for the treatment of process of palmitinic acid residue is provided;
The method, by processing the palmitinic acid residue produced in production process, not only avoid environment, and is recycled, significantly improve the yield of VC cetylate product, reduces production cost, becomes Fei Weibao.
The present invention is achieved through the following technical solutions:
The treatment process of palmitinic acid residue, is undertaken palmitinic acid residue-solvent rinse removal of impurities-centrifugal-airing-input xitix reacting-purify-crystallization-centrifugal-drying.
Preferably, after the solvent distillation obtained in described rotary process, solvent rinse removal of impurities operation recycling is returned.
Wherein, the material of described airing operation gained is the palmitinic acid raw material containing 80% ~ 90% palmitinic acid and 10% ~ 20%VC cetylate.
Preferably, solvent rinse removal of impurities operation: palmitinic acid residue is put in the first reactor, according to quality than palmitinic acid residue: ethyl acetate is that 1:5 ~ 10 add ethyl acetate, is fully uniformly mixed and obtains mixed slurry I;
Centrifugal, airing operation: mixed slurry I is carried out centrifugal treating, gained filter cake carries out airing and obtains material II, turns back in the first reactor after the distillation of gained filtrate;
Drop into xitix and carry out reaction process: be the amount of 5:3 with xitix according to mass ratio by material II, to put in the second reactor at 20 DEG C ~ 25 DEG C fully reaction 24 hours, obtain reaction mass III;
Purification process: first reaction mass III is carried out ice with ice and analyse, VC cetylate is separated out, then hexone, toluene is added, leave standstill after the VC cetylate of separating out dissolves completely, get rid of acid solution, leftover materials carry out crystallization, centrifugal, finally drop into ethyl acetate and carry out molten carrying, obtain material IV;
Crystallization Procedure: material IV is directly entered in container and leave standstill 24 ~ 36 hours.
Drying process: crystallization gains are carried out drying 1 ~ 3min with flash dryer, obtains VC cetylate.
Preferably, in purification process, described reaction mass III is 1:1.25 ~ 1.35 with the mass ratio of ice.
Preferably, in purification process, according to Mass Calculation, reactant: hexone: toluene: ethyl acetate=1:0.5:0.5:0.25.
Preferably, in purification process, described in add hexone and toluene is molten carries 25 ~ 35min, temperature is 60 DEG C ± 2, and stirring velocity is 25 ~ 35 turns/min.
Preferably, in purification process, ethyl acetate is molten carries 25 ~ 35min, and temperature is 60 DEG C ± 2, and stirring velocity is 25 ~ 35 turns/min.
Preferably, in drying process, flash dryer 1 ~ 3min, described flash dryer inlet temperature 110 DEG C ~ 125 DEG C, temperature out 78 DEG C ~ 85 DEG C.
The present invention first carries out rinse removal of impurities with solvent to palmitinic acid residue, then carry out reacting through centrifugal, airing, input xitix successively, purify, crystallization, centrifugal, dry operation the most at last palmitinic acid residue be converted into Quicifal, the solvent filtrate wherein obtained in rotary process returns rinse removal of impurities operation.One aspect of the present invention is prepared to tradition the waste residue that Quicifal produces and is processed, reduce the pollution to environment, on the other hand the useful matter in waste residue is extracted, become Fei Weibao, during Quicifal can be made to produce, product yield improves more than 10%, and cost reduces by 10% ~ 20%.
figure of description
Fig. 1 is technique of the present invention and schema.
concrete embodiment
Below in conjunction with embodiment, the present invention is described in further detail, understands the present invention to help those skilled in the art.
Embodiment 1
The treatment process of palmitinic acid residue, first puts in the first reactor by palmitinic acid residue, according to quality than palmitinic acid residue: ethyl acetate is that 1:10 adds ethyl acetate, is fully uniformly mixed and obtains mixed slurry I.Then, gained mixed slurry I is carried out centrifugal treating, gained filter cake carries out airing and obtains material II, turns back in the first reactor after the distillation of gained filtrate; Be the amount of 5:3 with xitix according to mass ratio by material II, to put in the second reactor fully reaction 24 hours, obtain reaction mass III, described temperature of reaction is 25 DEG C.Then, be first that 1:1.35 mixes by reaction mass III and the mass ratio of ice, carry out ice and analyse, VC cetylate is separated out, then add hexone, to carry out the molten 35min(of putting forward temperature be 60 DEG C ± 2 to toluene, stirring velocity is 35 turns/min), until after material dissolves completely, leave standstill, get rid of acid solution, residue feed liquid carries out crystallization, centrifugal, finally carries out molten carrying by ethyl acetate, obtains material IV; Material IV is directly entered normal temperature crystallization in great Bai bucket, crystallization time 36 hours.According to Mass Calculation, reactant: hexone: toluene: ethyl acetate=1:0.5:0.5:0.25.
Finally use flash dryer 3min, obtain VC cetylate.Described flash dryer inlet temperature 125 DEG C, temperature out 85 DEG C.
Embodiment 2
The treatment process of palmitinic acid residue, first puts in the first reactor by palmitinic acid residue, according to quality than palmitinic acid residue: ethyl acetate is that 1:7 adds ethyl acetate, is fully uniformly mixed and obtains mixed slurry I.Then, gained mixed slurry I is carried out centrifugal treating, gained filter cake carries out airing and obtains material II, turns back in the first reactor after the distillation of gained filtrate; Be the amount of 5:3 with xitix according to mass ratio by material II, to put in the second reactor fully reaction 24 hours, obtain reaction mass III, described temperature of reaction is 22 DEG C.Then, be first that 1:1.3 mixes by reaction mass III and the mass ratio of ice, carry out ice and analyse, VC cetylate is separated out, then add hexone, to carry out the molten 30min(of putting forward temperature be 60 DEG C ± 2 to toluene, stirring velocity is 30 turns/min), until after material dissolves completely, leave standstill, get rid of acid solution, residue feed liquid carries out crystallization, centrifugal, finally carries out molten carrying by ethyl acetate, obtains material IV; Material IV is directly entered normal temperature crystallization in great Bai bucket, crystallization time 30 hours.According to Mass Calculation, reactant: hexone: toluene: ethyl acetate=1:0.5:0.5:0.25.
Finally use flash dryer 2min, obtain VC cetylate.Described flash dryer inlet temperature 115 DEG C, temperature out 80 DEG C.
Embodiment 3
The treatment process of palmitinic acid residue, first puts in the first reactor by palmitinic acid residue, according to quality than palmitinic acid residue: ethyl acetate is that 1:5 adds ethyl acetate, is fully uniformly mixed and obtains mixed slurry I.Then, gained mixed slurry I is carried out centrifugal treating, gained filter cake carries out airing and obtains material II, turns back in the first reactor after the distillation of gained filtrate; Be the amount of 5:3 with xitix according to mass ratio by material II, to put in the second reactor fully reaction 24 hours, obtain reaction mass III, described temperature of reaction is 20 DEG C.Then, be first that 1:1.25 mixes by reaction mass III and the mass ratio of ice, carry out ice and analyse, VC cetylate is separated out, then add hexone, to carry out the molten 25min(of putting forward temperature be 60 DEG C ± 2 to toluene, stirring velocity is 25 turns/min), until after material dissolves completely, leave standstill, get rid of acid solution, residue feed liquid carries out crystallization, centrifugal, finally carries out molten carrying by ethyl acetate, obtains material IV; Material IV is directly entered normal temperature crystallization in great Bai bucket, crystallization time 24 hours.According to Mass Calculation, reactant: hexone: toluene: ethyl acetate=1:0.5:0.5:0.25.
Finally use flash dryer 1min, obtain VC cetylate.Described flash dryer inlet temperature 110 DEG C, temperature out 78 DEG C.
Above-described embodiment, just preferred embodiment of the present invention, is not used for limiting the scope of the present invention, therefore all equivalences done with the feature described in the claims in the present invention and principle change or modify, and all should be included within the claims in the present invention scope.
Claims (6)
- The preparation method of 1.VC cetylate, is characterized in that, treatment process is: and palmitinic acid residue-solvent rinse removal of impurities-the first be centrifugal-and airing-input xitix carries out reacting-purify-and crystallization-the second is centrifugal-dry;Be specially:Solvent rinse removal of impurities operation: palmitinic acid residue is put in the first reactor, according to quality than palmitinic acid residue: ethyl acetate is that 1:5 ~ 10 add ethyl acetate, is fully uniformly mixed and obtains mixed slurry I;Centrifugal, airing operation: mixed slurry I is carried out centrifugal treating, gained filter cake carries out airing and obtains material II, turns back in the first reactor after the distillation of gained filtrate;Drop into xitix and carry out reaction process: be the amount of 5:3 with xitix according to mass ratio by material II, put in the second reactor, at 20 DEG C ~ 25 DEG C, fully reaction 24 hours, obtains reaction mass III;Purification process: first reaction mass III is carried out ice with ice and analyse, VC cetylate is separated out, then hexone, toluene is added, leave standstill after the VC cetylate of separating out dissolves completely, get rid of acid solution, leftover materials carry out crystallization, centrifugal, finally drop into ethyl acetate and carry out molten carrying, obtain material IV;Crystallization Procedure: material IV is directly entered in container and leave standstill 24 ~ 36 hours.Drying process: crystallization gains are carried out drying 1 ~ 3min with flash dryer, obtains VC cetylate;Wherein, described palmitinic acid residue is: chemical process prepares the palmitinic acid residue produced in food antioxidant vitamin-c palmitate process; The material of described airing operation gained is the palmitinic acid raw material containing 80% ~ 90% palmitinic acid and 10% ~ 20%VC cetylate.
- 2. the preparation method of VC cetylate as claimed in claim 1, is characterized in that, in purification process, described reaction mass III is 1:1.25 ~ 1.35 with the mass ratio of ice.
- 3. the preparation method of VC cetylate as claimed in claim 1, is characterized in that, in purification process, according to Mass Calculation, and reactant: hexone: toluene: ethyl acetate=1:0.5:0.5:0.25.
- 4. the preparation method of VC cetylate as claimed in claim 1, is characterized in that, in purification process, described in add hexone and toluene is molten carries 25 ~ 35min, temperature is 60 DEG C ± 2, and stirring velocity is 25 ~ 35 turns/min.
- 5. the preparation method of VC cetylate as claimed in claim 1, it is characterized in that, in purification process, ethyl acetate is molten carries 25 ~ 35min, and temperature is 60 DEG C ± 2, and stirring velocity is 25 ~ 35 turns/min.
- 6. the preparation method of VC cetylate as claimed in claim 1, is characterized in that, in drying process, and flash dryer 1 ~ 3min, described flash dryer inlet temperature 110 DEG C ~ 125 DEG C, temperature out 78 DEG C ~ 85 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108569963A (en) * | 2018-05-02 | 2018-09-25 | 广东广益科技实业有限公司 | A kind of production technology of palmitic acid waste residue recycling |
| CN113372312A (en) * | 2021-07-01 | 2021-09-10 | 江西凯泰食品科技有限公司 | Environment-friendly ascorbyl palmitate and production method thereof |
Citations (6)
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| CN1394856A (en) * | 2001-07-10 | 2003-02-05 | 陕西渭南生物生化专利技术研究所 | Process and formula for synthesizing L-ascorbyl palmitate |
| CN102260231A (en) * | 2009-07-25 | 2011-11-30 | 邓志中 | Preparation method of ascorbyl palmitate |
| CN102532071A (en) * | 2011-09-05 | 2012-07-04 | 浙江天新药业有限公司 | L-ascorbyl palmitate particles, and preparation method and application thereof |
| CN102558115A (en) * | 2011-12-29 | 2012-07-11 | 蚌埠丰原医药科技发展有限公司 | Preparation method of L-ascorbyl palmitate |
| CN102304109B (en) * | 2011-08-29 | 2013-06-26 | 河北维尔康制药有限公司 | Method for synthesizing L-ascorbyl palmitate |
| CN103254160A (en) * | 2013-05-20 | 2013-08-21 | 东北制药集团股份有限公司 | Method for separating and purifying vitamin C palmitate from reaction liquid of direct esterification method |
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- 2013-12-24 CN CN201310720183.XA patent/CN103739580B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394856A (en) * | 2001-07-10 | 2003-02-05 | 陕西渭南生物生化专利技术研究所 | Process and formula for synthesizing L-ascorbyl palmitate |
| CN102260231A (en) * | 2009-07-25 | 2011-11-30 | 邓志中 | Preparation method of ascorbyl palmitate |
| CN102304109B (en) * | 2011-08-29 | 2013-06-26 | 河北维尔康制药有限公司 | Method for synthesizing L-ascorbyl palmitate |
| CN102532071A (en) * | 2011-09-05 | 2012-07-04 | 浙江天新药业有限公司 | L-ascorbyl palmitate particles, and preparation method and application thereof |
| CN102558115A (en) * | 2011-12-29 | 2012-07-11 | 蚌埠丰原医药科技发展有限公司 | Preparation method of L-ascorbyl palmitate |
| CN103254160A (en) * | 2013-05-20 | 2013-08-21 | 东北制药集团股份有限公司 | Method for separating and purifying vitamin C palmitate from reaction liquid of direct esterification method |
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