CN109111423A - A kind of method that crude glycerine recycling prepares solketal - Google Patents
A kind of method that crude glycerine recycling prepares solketal Download PDFInfo
- Publication number
- CN109111423A CN109111423A CN201810508320.6A CN201810508320A CN109111423A CN 109111423 A CN109111423 A CN 109111423A CN 201810508320 A CN201810508320 A CN 201810508320A CN 109111423 A CN109111423 A CN 109111423A
- Authority
- CN
- China
- Prior art keywords
- crude glycerine
- solketal
- added
- acetone
- acid
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/14—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D317/18—Radicals substituted by singly bound oxygen or sulfur atoms
- C07D317/20—Free hydroxyl or mercaptan
Abstract
A kind of method that crude glycerine recycling prepares solketal is related to the technology field that a kind of chemical method prepares solketal using crude glycerine.First crude glycerine pickling to faintly acid, crude glycerine is isolated in filtering, treated, and crude glycerine pours into reaction kettle, and acetone is added, and the concentrated sulfuric acid is added, add the imitative Soxhlet extractor water removal of desiccant, is back to after reaction, reduces temperature to 50 DEG C, alkali neutralization is added, adjusts pH=6.5, filtering, obtain filtrate, it is distilled to recover acetone, then is evaporated under reduced pressure out solketal, product purity is up to 99%.
Description
Technical field
The present invention relates to the processes that a kind of chemical synthesis process, especially crude glycerine recycling prepare solketal.
Background technique
Along with the constantly development of oil prodution industry, more and more crude glycerines generate therewith.Processing to crude glycerine and
Using the processing mode of crude glycerine generally has following several at present: 1. refined glycerines, but it is refined into pure glycerin.Generally to sweet
The most common method of purification and the highest method of product quality of oil are exactly to be evaporated under reduced pressure.Glycerol is by being evaporated under reduced pressure out
The fraction of 180-190 DEG C (1kpa), then by active carbon decoloring, deodorization can be obtained pure glycerol.Wherein due to glycerol
Property is special, is purified by vacuum distillation, and it is all more wasteful resource that either raising vacuum degree, which still improves temperature,.2.
It is 1,2-PD or 1,3-PD by hydrogenating reduction, it is not selectively too high for restoring to glycerol, so to be referred to
Fixed product is generally with dedicated catalyst.Under normal circumstances, some compound noble metal catalysts be will use, it is compound
Catalyst of transition metal oxide etc..The price of these catalyst is higher, and production technology is complicated.3. being prepared by bioanalysis
Lactic acid.Bioanalysis is although simple and easy, but since its requirement to technological parameter is relatively high, and bioanalysis consumption energy can be led
The loss of material is caused, and is also easy to produce by-product, hardly possible separation.These methods have waste of resource, complex process, at high cost, by-product
The various disadvantages such as hardly possible separation.
Summary of the invention
Object of the present invention is to propose a kind of method that environmentally friendly, efficient crude glycerine recycling prepares solketal.
The present invention the following steps are included:
1. a kind of method that crude glycerine recycling prepares solketal, it is characterised in that the following steps are included:
1) sulfuric acid solution (or one of phosphoric acid, hydrochloric acid) is added to crude glycerine, is adjusted to pH=6, filter, isolate thick sweet
Oil.
2) crude glycerine is poured into reaction kettle, acetone is added in reaction kettle, the concentrated sulfuric acid is added, add desiccant with imitative Soxhlet extractor
Water removal is back to after reaction, is reduced temperature to 50 DEG C, is added alkali (one of sodium carbonate, sodium bicarbonate, sodium hydroxide)
PH=6.5 are adjusted, filtering obtains filtrate, is distilled to recover acetone, then be evaporated under reduced pressure out solketal.
The sulfuric acid solution concentration is 7~10mol/L's
The desiccant is one of anhydrous sodium sulfate, anhydrous magnesium sulfate；
The alkali is one of sodium carbonate, sodium bicarbonate, sodium hydroxide；
The addition acetone feeds intake to be added by the mass ratio of the material (glycerol: acetone=1:3~6)；
In the step 2,6% that concentrated sulfuric acid amount is qualities of glycerin is added；
In the step 2, adding desiccant dosage anhydrous sodium sulfate is the 3~8% of acetone quality.
Detailed description of the invention
Fig. 1 is the reacting flow chart of technique
Specific embodiment
Step 1: crude glycerine pickling
100mL crude glycerine is added in 250 mL beakers, the sulfuric acid solution of 9mol/L is added, is adjusted to pH=6, filters, isolates
Crude glycerine.
Step 2: the preparation of solketal
The crude glycerine of step 1 is poured into 1000mL round-bottomed flask, 390mL acetone is then added, the 8mL concentrated sulfuric acid is added, is added 5
The imitative Soxhlet extractor water removal of gram anhydrous sodium sulfate, 80 DEG C are flowed back 6 hours.After reaction, reducing temperature is 50 DEG C, and carbon is added
Sour sodium is adjusted to pH=6.5, and filtering obtains filtrate, is distilled to recover acetone, then be evaporated under reduced pressure out solketal.
The reaction mechanism is as follows for it:
Claims (6)
1. a kind of method that crude glycerine recycling prepares solketal, it is characterised in that the following steps are included:
1) in crude glycerine, pH is adjusted with acid to faintly acid, crude glycerine is isolated in filtering；
2) crude glycerine is poured into reaction kettle, acetone is added in reaction kettle, concentrated acid is added, desiccant is added to be removed with imitative Soxhlet extractor
Water is back to after reaction, reduces temperature to 50 DEG C, and alkali is added and adjusts pH value, and filtering obtains filtrate, is distilled to recover acetone, then
It is evaporated under reduced pressure out solketal.
The acid is one of sulfuric acid, phosphoric acid, hydrochloric acid；
The desiccant is one of anhydrous sodium sulfate, anhydrous magnesium sulfate；
The alkali is one of sodium carbonate, sodium bicarbonate, sodium hydroxide.
2. a kind of method that crude glycerine recycling prepares solketal according to claim 1, it is characterised in that the step
1) in, crude glycerine is added in a kettle, is adjusted with acid pH to 6, filters, isolates crude glycerine.
3. a kind of method that crude glycerine recycling prepares solketal according to claim 1, it is characterised in that the step
2) in, acetone is added and presses the mass ratio of the material (glycerol: acetone=1:3~6).
4. a kind of method that crude glycerine recycling prepares solketal according to claim 1, it is characterised in that the step
2) in, 5~10% that concentrated acid amount is qualities of glycerin are added.
5. a kind of method that crude glycerine recycling prepares solketal according to claim 1, it is characterised in that the step
2) in, adding desiccant dosage anhydrous sodium sulfate is the 3-8% of acetone quality.
6. a kind of method that crude glycerine recycling prepares solketal according to claim 1, it is characterised in that the step
2) in, alkali (sodium carbonate) is added and adjusts pH value to pH=6.5, filtering obtains filtrate, is distilled to recover acetone, then be evaporated under reduced pressure out acetone
Contracting glycerol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810508320.6A CN109111423A (en) | 2018-05-24 | 2018-05-24 | A kind of method that crude glycerine recycling prepares solketal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810508320.6A CN109111423A (en) | 2018-05-24 | 2018-05-24 | A kind of method that crude glycerine recycling prepares solketal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109111423A true CN109111423A (en) | 2019-01-01 |
Family
ID=64822735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810508320.6A Pending CN109111423A (en) | 2018-05-24 | 2018-05-24 | A kind of method that crude glycerine recycling prepares solketal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109111423A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111848343A (en) * | 2020-08-11 | 2020-10-30 | 深圳飞扬兴业科技有限公司 | Process and device for refining glycerol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102066297A (en) * | 2008-05-19 | 2011-05-18 | 罗狄亚聚酰胺特殊品有限公司 | Method of purifying crude glycerol |
| CN102226134A (en) * | 2011-05-12 | 2011-10-26 | 福建漳州鼎能生物科技有限公司 | Method for producing biodiesel by using waste oil |
| CN103842351A (en) * | 2011-09-30 | 2014-06-04 | 罗狄亚聚酰胺特殊品有限公司 | Process for the production of a dioxolane compound from crude glycerol including a liquid-liquid extraction step |
-
2018
- 2018-05-24 CN CN201810508320.6A patent/CN109111423A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102066297A (en) * | 2008-05-19 | 2011-05-18 | 罗狄亚聚酰胺特殊品有限公司 | Method of purifying crude glycerol |
| CN102226134A (en) * | 2011-05-12 | 2011-10-26 | 福建漳州鼎能生物科技有限公司 | Method for producing biodiesel by using waste oil |
| CN103842351A (en) * | 2011-09-30 | 2014-06-04 | 罗狄亚聚酰胺特殊品有限公司 | Process for the production of a dioxolane compound from crude glycerol including a liquid-liquid extraction step |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111848343A (en) * | 2020-08-11 | 2020-10-30 | 深圳飞扬兴业科技有限公司 | Process and device for refining glycerol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102757308B (en) | Method of preparing high-purity ethanol | |
| CN101102986B (en) | Method for preparing trimethylolpropane | |
| CN101089009A (en) | Diosmin producing process | |
| CN101274892B (en) | Method for preparing L-menthol glyoxylic ester monohydrate with solid acid as catalyst | |
| CN105601481B (en) | The method that a kind of ozone cooperative heterogeneous catalysis cinnamic acid or cinnamon oil prepare natural benzaldehyde | |
| CN109111423A (en) | A kind of method that crude glycerine recycling prepares solketal | |
| CN103387593B (en) | A kind of method of coproduction maltonic acid-delta-lactone, seminose and N.F,USP MANNITOL | |
| CN110015943A (en) | A kind of preparation method of nervonic acid | |
| CN103214421B (en) | The industrialized preparing process of 2-sulfydryl-1-Methylimidazole | |
| CN108191690A (en) | The energy-saving and environment-friendly continuous preparation method of Iohexol | |
| CA2914316A1 (en) | Process for producing polyhydric alcohol | |
| CN103497214A (en) | Clean preparation method of ethyl chloride with high purity | |
| CN103804205B (en) | A kind of technique preparing o-aminophenol | |
| CN101973870B (en) | Preparation of glycollic acid from oxalaldehyde by intramolecular disproportionation method | |
| CN102417178A (en) | Method for removing polyphosphate from activated carbon of phosphoric acid method | |
| CN102408329A (en) | Preparation method of 2,4-dihydroxy benzoic acid | |
| CN103420882B (en) | A kind of preparation method of L-Methionine | |
| CN108299186B (en) | Novel synthesis process of propoxyacetic acid | |
| CN101759582A (en) | New process for producing DL-p-hydroxyphenylglycine | |
| WO2007073240A1 (en) | Catalyst, a method for the production thereof and a dihydroxyalkane production method | |
| CN111875666B (en) | Method for synthesizing Edwarden sweet | |
| CN1569819A (en) | Process for synthesizing paracetamol | |
| CN114890869B (en) | Refining and deodorizing method for 1, 3-butanediol | |
| CN102746260A (en) | Method for preparing benzofuran-2-(3H)-one | |
| CN101823948A (en) | Method for co-producing methyl chloride with chloroactic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190101 |
|
| WD01 | Invention patent application deemed withdrawn after publication |