CN103739580A - Treatment method of palmitic acid residues - Google Patents
Treatment method of palmitic acid residues Download PDFInfo
- Publication number
- CN103739580A CN103739580A CN201310720183.XA CN201310720183A CN103739580A CN 103739580 A CN103739580 A CN 103739580A CN 201310720183 A CN201310720183 A CN 201310720183A CN 103739580 A CN103739580 A CN 103739580A
- Authority
- CN
- China
- Prior art keywords
- palmitinic acid
- acid residue
- treatment process
- ethyl acetate
- centrifugal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of industry engineering, and particularly relates to a treatment method of palmitic acid residues generated in the technological process of ascorbyl palmitate production. The treatment method comprises the following steps: firstly using a solvent for moistening and washing the palmitic acid residues so as remove impurities in the palmitic acid residues, then sequentially carrying out working procedures such as centrifuging, airing, putting ascorbic acids for reaction, purifying, crystallizing and drying, and finally converting the palmitic acid residues to the ascorbyl palmitate, wherein solvent filtrate obtained in the centrifuging working procedure returns to the moistening and washing impurity removal working procedure. The treatment method has the advantages that waste residues generated in a traditional preparation process of the ascorbyl palmitate are treated and prevented from polluting environments on the one hand, useful materials in the waste residues are utilized on the other hand, so that waste is turned into wealth, the yield of products in the ascorbyl palmitate production is increased by above 10%, and the cost is reduced 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 producing in Quicifal production process.
Background technology
Quicifal (being also VC cetylate) is that the natural component esterifications such as palmitinic acid and L-AA form, and its molecular formula is C
22h
38o
7, be a kind of oxygen scavenqer and synergistic agent efficiently, by the foodstuff additive council of the World Health Organization (WHO) be assessed as there is trophicity, nontoxic, efficient, use safe foodstuff additive.
At present, the preparation method of food antioxidant Quicifal mainly contains chemical process and biological method, and wherein chemical process mainly makes through a series of esterifications, purification with raw material xitix, palmitinic acid.In production process, in order to reach best product yield, palmitinic acid is excessive input, causes producing a large amount of palmitinic acid residue (in residue approximately 80%～90% be Quicifal and other impurity on a small quantity for palmitinic acid, 10%～20%).In existing explained hereafter, waste residue is not all used and not only causes raw material to waste, and cause environmental pollution.
Summary of the invention
In order to address the above problem, the object of the invention is to, a kind for the treatment of process of palmitinic acid residue is provided;
The method is processed by the palmitinic acid residue to producing in production process, has not only avoided environment, and has been recycled, and obviously improves the yield of VC cetylate product, reduces production costs, and becomes Fei Weibao.
The present invention is achieved through the following technical solutions:
The treatment process of palmitinic acid residue, reacts palmitinic acid residue-solvent rinse removal of impurities-centrifugal-airing-input xitix-purify-crystallization-be centrifugal-dry.
Preferably, after the solvent distillation obtaining in described rotary process, return to solvent rinse removal of impurities operation recycling.
Wherein, the material of described airing operation gained is the palmitinic acid raw material that contains 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 to centrifugal treating, and gained filter cake carries out airing and obtains material II, turn back in the first reactor after the distillation of gained filtrate;
Drop into xitix and carry out reaction process: the amount that is 5:3 according to mass ratio by material II and xitix, put in the second reactor and fully react 24 hours at 20 ℃～25 ℃, obtain reaction mass III;
Purification process: first reaction mass III is carried out to ice with ice and analyse, VC cetylate is separated out, then add hexone, toluene, it is standing 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, and obtain material IV;
Crystallization Procedure: material IV is directly entered in container to standing 24～36 hours.
Drying process: crystallization gains are dried to 1～3min with flash dryer, obtain VC cetylate.
Preferably, in purification process, the mass ratio of described reaction mass III and ice is 1:1.25～1.35.
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 the molten 25～35min that carries of toluene, temperature is 60 ℃ ± 2, stirring velocity is 25～35 turn/min.
Preferably, in purification process, the molten 25～35min that carries of ethyl acetate, temperature is 60 ℃ ± 2, stirring velocity is 25～35 turn/min.
Preferably, in drying process, flash dryer 1～3min, 110 ℃～125 ℃ of described flash dryer inlet temperatures, 78 ℃～85 ℃ of temperature outs.
The present invention first carries out rinse removal of impurities with solvent to palmitinic acid residue, then successively through centrifugal, airing, input xitix react, purification, crystallization, centrifugal, dry operation the most at last palmitinic acid residue be converted into Quicifal, the solvent filtrate wherein obtaining in rotary process is returned to rinse removal of impurities operation.One aspect of the present invention is prepared to tradition the waste residue that Quicifal produces and is processed, reduced the pollution to environment, on the other hand the useful matter in waste residue is extracted, become Fei Weibao, can make product yield in Quicifal production improve more than 10%, cost 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, to help those skilled in the art, understands the present invention.
Embodiment 1
The treatment process of palmitinic acid residue, first puts into palmitinic acid residue in the first reactor, 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 to centrifugal treating, gained filter cake carries out airing and obtains material II, after the distillation of gained filtrate, turns back in the first reactor; The amount that is 5:3 according to mass ratio by material II and xitix, puts in the second reactor fully reaction 24 hours, obtains reaction mass III, and described temperature of reaction is 25 ℃.Then, by reaction mass III and the mass ratio of ice, be first that 1:1.35 mixes, carry out ice and analyse, VC cetylate is separated out, then adding hexone, toluene to carry out the molten 35min(of putting forward temperature is 60 ℃ ± 2, stirring velocity is 35 turn/min), until after material dissolves completely, standing, get rid of acid solution, residue feed liquid is carried out crystallization, centrifugal, finally by ethyl acetate, carries out molten carrying, and obtains material IV; Material IV is directly entered to 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.125 ℃ of described flash dryer inlet temperatures, 85 ℃ of temperature outs.
Embodiment 2
The treatment process of palmitinic acid residue, first puts into palmitinic acid residue in the first reactor, 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 to centrifugal treating, gained filter cake carries out airing and obtains material II, after the distillation of gained filtrate, turns back in the first reactor; The amount that is 5:3 according to mass ratio by material II and xitix, puts in the second reactor fully reaction 24 hours, obtains reaction mass III, and described temperature of reaction is 22 ℃.Then, by reaction mass III and the mass ratio of ice, be first that 1:1.3 mixes, carry out ice and analyse, VC cetylate is separated out, then adding hexone, toluene to carry out the molten 30min(of putting forward temperature is 60 ℃ ± 2, stirring velocity is 30 turn/min), until after material dissolves completely, standing, get rid of acid solution, residue feed liquid is carried out crystallization, centrifugal, finally by ethyl acetate, carries out molten carrying, and obtains material IV; Material IV is directly entered to 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.115 ℃ of described flash dryer inlet temperatures, 80 ℃ of temperature outs.
Embodiment 3
The treatment process of palmitinic acid residue, first puts into palmitinic acid residue in the first reactor, 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 to centrifugal treating, gained filter cake carries out airing and obtains material II, after the distillation of gained filtrate, turns back in the first reactor; The amount that is 5:3 according to mass ratio by material II and xitix, puts in the second reactor fully reaction 24 hours, obtains reaction mass III, and described temperature of reaction is 20 ℃.Then, by reaction mass III and the mass ratio of ice, be first that 1:1.25 mixes, carry out ice and analyse, VC cetylate is separated out, then adding hexone, toluene to carry out the molten 25min(of putting forward temperature is 60 ℃ ± 2, stirring velocity is 25 turn/min), until after material dissolves completely, standing, get rid of acid solution, residue feed liquid is carried out crystallization, centrifugal, finally by ethyl acetate, carries out molten carrying, and obtains material IV; Material IV is directly entered to 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.110 ℃ of described flash dryer inlet temperatures, 78 ℃ of temperature outs.
Above-described embodiment, is preferred embodiment of the present invention, is not used for limiting the scope of the present invention, and the equivalence of being done with the feature described in the claims in the present invention and principle therefore all changes or modifies, within all should being included in the claims in the present invention scope.
Claims (9)
1. the treatment process of palmitinic acid residue, is characterized in that, treatment process is: palmitinic acid residue-solvent rinse removal of impurities-centrifugal-airing-input xitix reacts-purifies-and crystallization-centrifugal-dry.
2. the treatment process of palmitinic acid residue as claimed in claim 1, is characterized in that, after the solvent distillation obtaining, returns to solvent rinse removal of impurities operation recycling in described rotary process.
3. the treatment process of palmitinic acid residue as claimed in claim 2, is characterized in that, the material of described airing operation gained, for containing the palmitinic acid raw material of 80%～90% palmitinic acid and 10%～20%VC cetylate.
4. the treatment process of palmitinic acid residue as claimed in claim 3, is characterized in that, is 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 to centrifugal treating, and gained filter cake carries out airing and obtains material II, turn back in the first reactor after the distillation of gained filtrate;
Drop into xitix and carry out reaction process: the amount that is 5:3 according to mass ratio by material II and xitix, put in the second reactor, at 20 ℃～25 ℃, fully react 24 hours, obtain reaction mass III;
Purification process: first reaction mass III is carried out to ice with ice and analyse, VC cetylate is separated out, then add hexone, toluene, it is standing 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, and obtain material IV;
Crystallization Procedure: material IV is directly entered in container to standing 24～36 hours.
Drying process: crystallization gains are dried to 1～3min with flash dryer, obtain VC cetylate.
5. the treatment process of palmitinic acid residue as claimed in claim 4, is characterized in that, in purification process, the mass ratio of described reaction mass III and ice is 1:1.25～1.35.
6. the treatment process of palmitinic acid residue as claimed in claim 4, is characterized in that, in purification process, and according to Mass Calculation, reactant: hexone: toluene: ethyl acetate=1:0.5:0.5:0.25.
7. the treatment process of palmitinic acid residue as claimed in claim 4, is characterized in that, in purification process, described in add hexone and the molten 25～35min that carries of toluene, temperature is 60 ℃ ± 2, stirring velocity is 25～35 turn/min.
8. the treatment process of palmitinic acid residue as claimed in claim 4, is characterized in that, in purification process, and the molten 25～35min that carries of ethyl acetate, temperature is 60 ℃ ± 2, stirring velocity is 25～35 turn/min.
9. the treatment process of palmitinic acid residue as claimed in claim 4, is characterized in that, in drying process, and flash dryer 1～3min, 110 ℃～125 ℃ of described flash dryer inlet temperatures, 78 ℃～85 ℃ of temperature outs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310720183.XA CN103739580B (en) | 2013-12-24 | 2013-12-24 | The treatment process of palmitinic acid residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310720183.XA CN103739580B (en) | 2013-12-24 | 2013-12-24 | The treatment process of palmitinic acid residue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103739580A true CN103739580A (en) | 2014-04-23 |
| CN103739580B CN103739580B (en) | 2016-04-20 |
Family
ID=50496668
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310720183.XA Active CN103739580B (en) | 2013-12-24 | 2013-12-24 | The treatment process of palmitinic acid residue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103739580B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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)
| 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 |
| 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 |
-
2013
- 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103739580B (en) | 2016-04-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106565973A (en) | Preparation method of mineral-based fulvic acid | |
| CN102010318B (en) | Production method of mixed long carbon chain dibasic acid | |
| US2189376A (en) | Method of producing aluminium oxide from aluminiferous raw materials | |
| CN110877914A (en) | Method for preparing high-purity high-white calcium carbonate by mineralizing and fixing carbon dioxide with phosphogypsum | |
| CN103264991B (en) | Method for processing sulfur paste as coke oven gas desulfuration by-product | |
| CN103739580A (en) | Treatment method of palmitic acid residues | |
| CN103896307A (en) | Method for refining coke oven gas desulfurization waste liquid salt extraction product ammonium sulfate again | |
| CN101891164B (en) | Method for purifying cubic boron nitride | |
| CN101555238A (en) | Method for tetrahydrofuran recycling | |
| CN115504695B (en) | Phosphogypsum recycling method | |
| CN103772330B (en) | Method for recovery of furfural and acetic acid from furfural stripping steam condensate | |
| CN101531582A (en) | Method for preparing sodium diacetate by industrial waste | |
| NL2024457B1 (en) | Method for simultaneously recovering furfural product and sulfuric acid catalyst from furfural residue | |
| CN102964252A (en) | Technology for preparing propyl gallate by utilizing mixed catalyst | |
| CN102115358A (en) | Method for producing pentaerythritol and sodium formate with waste liquor generated during preparation of pentaerythritol | |
| CN1235862C (en) | Technique for esterification synthesizing propyl gallate without water added | |
| CN105294642B (en) | A kind of method that catalyzing glycerol prepares chemical products | |
| CN102912141A (en) | Method for digesting waste rhodium catalyst from olefin hydroformylation reaction | |
| CN106698479A (en) | Non-aqueous complete-dissolution refining method of sodium fluoride containing organic impurities | |
| CN106431506A (en) | Nitrogen fertilizer containing amide nitrogen and nitrate nitrogen and method for treating concentrated nitric acid contained wastewater | |
| CN1651390A (en) | Method of preparing adipic acid by cyclohexane oxidation liquid pickling water HzO2 catalytic oxidation | |
| CN108569963A (en) | A kind of production technology of palmitic acid waste residue recycling | |
| CN102115382A (en) | Method for producing co-product of pentaerythritol as well as ammonium formate and sodium sulfate by waste liquid generated by preparation of pentaerythritol | |
| CN103992256A (en) | Method for preparing high-purity lutein esters from pot marigold | |
| CN1196340A (en) | High-efficiency boron-magnesium fertilizer and producing method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |