CN101070269A - Ester exchange method for producing pure glycerin from coarse glycerin - Google Patents
Ester exchange method for producing pure glycerin from coarse glycerin Download PDFInfo
- Publication number
- CN101070269A CN101070269A CN 200610020997 CN200610020997A CN101070269A CN 101070269 A CN101070269 A CN 101070269A CN 200610020997 CN200610020997 CN 200610020997 CN 200610020997 A CN200610020997 A CN 200610020997A CN 101070269 A CN101070269 A CN 101070269A
- Authority
- CN
- China
- Prior art keywords
- ester
- raw material
- insert
- pressurized air
- retort
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
This invention relates to manufacturing method of a net glycerol, especially use raw glycerine to process net glyceric by olein ester exchanging method. First use vitriol to acidify the ester exchanging raw glycerine, then put in reaction tank and adopt agent for disposing, at the same time inlet compressed air, then vacuum concentration and cyclic degas for dryness, at last use molecular distillation apparatus to distil, then decolour, the distillation temperature is controlled at 120 to 130deg, vacuum degree controlled at 1 to 5Pa. The glycerol purification could reach 99.5%upwards, the fatty acid, fat, and heavy metal ion of the finished product satisfy standards. The invention is suitable for large-scale industry production.
Description
(1) technical field
The present invention relates to a kind of production method of ester-interchange method raw glycerine processing pure glycerin, particularly a kind of production method of utilizing stearic exchange process raw glycerine processing pure glycerin.
(2) background technology
The content of glycerine is 40%-70% in the stearic exchange process by-product sugar water, wherein contains a large amount of formicesters, pigment, colloid and other impurity.With stearic exchange process by-product sugar water is that raw material generally is manufacture glycerine (purity about 95%), and added value of product is low.Utilize the technology of ion exchange resin processing pure glycerin, though be effectively technically, because the cost issues that resin regeneration and waste resin are handled is not suitable for large-scale commercial production.General continuous processing pure glycerin production technique, also needs falling-film evaporator to remove residue and reclaims glycerine except that still kettle in distillation workshop section, and the glycerine that condenser condenses is got off also needs the deodorizing operation just can enter bleacher, needs equipment many, the production cost height, and power consumption is big.
(3) summary of the invention
The objective of the invention is to overcome above-mentioned prior art deficiency, a kind of large-scale commercial production that is suitable for is provided, technology is simple, and production cost is low, the production method of the ester-interchange method raw glycerine processing pure glycerin that energy consumption is little.
Solution of the present invention is: a kind of production method of ester-interchange method raw glycerine processing pure glycerin is characterized in carrying out according to the following steps:
A, with ester-interchange method raw glycerine sulfuric acid acidation;
Insert after b, the acidifying and adopt chemicals treatment in the retort, and feed pressurized air;
Circulating degasification drying behind c, the vacuum concentration;
D, with decolouring again after the molecular still distillation, wherein distillation temperature is controlled at 120-130 ℃, vacuum control is at 1-5Pa in the distiller.
Raw material acidifying purpose is to make unreacted grease to separate from raw material among the present invention, is convenient to remove grease and ester.The purpose of chemicals treatment is to remove formicester, colloid, pigment and various heavy metal ion and acidifying SO
4 2-In the chemicals treatment process, the medicament of not removing in the glycerine will be removed in still-process.
Sulfuric acid acidation makes the raw material pH value be adjusted into 5-6.5 in the terms of settlement of the present invention, and acidificatoin time is 1-1.5 hour, and temperature is controlled at 80-90 ℃.
Chemicals treatment can adopt to insert after the acidifying and be heated to 90-100 ℃ in the retort in the terms of settlement of the present invention, the calcium oxide or the calcium hydroxide that add raw material weight 1.5-3.5%, and feeding pressurized air, behind the pressure filter circulating filtration, insert and be heated to 90-100 ℃ in another retort, the hydrated barta that adds raw material weight 1-2% again, add oxalate then, and feed pressurized air.Adding calcium oxide or calcium hydroxide purpose is to remove free fatty acids and most of SO
4 2-, impurity such as precipitation absorption that utilization generates and sedimentation formicester, colloid, pigment.Add hydrated barta to remove SO
4 2-, utilize barium sulfate further to precipitate adsorpting pigment.Add oxalic acid or oxalate, remove calcium, barium ion and other heavy metal ion.Feed pressurized air except that stirring, another purpose is to utilize the gas come-up to take the oily foam of suspension out of, is convenient to remove the grease of trace.Oxalic acid or oxalate will be removed in still-process.
Advantage of the present invention: the present invention can effectively remove impurity such as formicesters a large amount of in the ester-interchange method raw glycerine, colloid, pigment, raw glycerine is purified to more than 99.5%, lipid acid and ester, heavy metal ion satisfy standard in the finished product glycerine, and technology is simple, production cost is low, energy consumption is little, is applicable to large-scale commercial production.
(4) embodiment
The embodiment of the invention is as follows: with the vitriol oil acidifying of stearic exchange process by-product sugar water, adjust the raw material pH value and reach 6, acidificatoin time is 1 hour 20 minutes, and temperature is controlled at 85 ℃, and the sugar water after the acidifying is inserted and is heated to 90-95 ℃ in the retort, the calcium oxide that adds raw material weight 2%, feed pressurized air simultaneously, behind the pressure filter circulating filtration, insert and be heated to 90-95 ℃ in another retort, add the hydrated barta that accounts for raw material weight 1.5%, feed pressurized air simultaneously, add oxalic acid afterwards again; Vacuum concentration divides two sections to carry out, and first section sugar water boiling temperature is controlled at 85-95 ℃, vacuum tightness 70Kpa, and second section sugar water boiling temperature is controlled at 65-75 ℃, and vacuum tightness 10Kpa obtains the raw glycerine of content 88%-93%; The raw glycerine that obtains is sloughed moisture by the circulating degasification drying, send into the molecular distillation equipment distillation again, 125 ℃ of control distillation temperatures, vacuum tightness 4Pa; Directly send into the bleacher decolouring from the glycerine that molecular still obtains, obtain the finished product pure glycerin.The every after tested index of the resultant pure glycerin of present embodiment is as follows: glycerol content 99.57%, colourity (hazen) 5, muriate (CL%)＜0.002, vitriol (SO
4 2-%)＜0.002, lipid acid that contains in acidity or alkalinity (mol/100g)＜0.0018, saponification equivalent (mol/100g)＜0.08, arsenic content (mg/kg)＜2, heavy metal content (mg/kg)＜2, the 40g pure glycerin and lipid consume 0.1mol/1NaOH0.45ml.
Claims (4)
1, a kind of production method of ester-interchange method raw glycerine processing pure glycerin is characterized in that carrying out according to the following steps:
A, with ester-interchange method raw glycerine sulfuric acid acidation;
Insert after b, the acidifying and adopt chemicals treatment in the retort, and feed pressurized air;
Circulating degasification drying behind c, the vacuum concentration;
D, with decolouring again after the molecular still distillation, wherein distillation temperature is controlled at 120-130 ℃, vacuum control is at 1-5Pa in the distiller.
2, the production method of ester-interchange method raw glycerine processing pure glycerin according to claim 1 is characterized in that it is 5-6.5 that sulfuric acid acidation makes the raw material pH value, and acidificatoin time is 1-1.5 hour, and temperature is controlled at 80-90 ℃.
3, the production method of ester-interchange method raw glycerine processing pure glycerin according to claim 1, it is characterized in that chemicals treatment adopts to insert after the acidifying is heated to 90-100 ℃ in the retort, the calcium oxide that adds raw material weight 1.5-3.5%, feeding pressurized air simultaneously stirs, behind the pressure filter circulating filtration, insert and be heated to 90-100 ℃ in another retort, the hydrated barta that adds raw material weight 1-2% again adds oxalate then, feeds pressurized air simultaneously and stirs.
4, the production method of ester-interchange method raw glycerine processing pure glycerin according to claim 1, it is characterized in that chemicals treatment adopts to insert after the acidifying is heated to 90-100 ℃ in the retort, the calcium hydroxide that adds raw material weight 1.5-3.5%, feeding pressurized air simultaneously stirs, behind the pressure filter circulating filtration, insert and be heated to 90-100 ℃ in another retort, the hydrated barta that adds raw material weight 1-2% again adds oxalate then, feeds pressurized air simultaneously and stirs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610020997 CN101070269A (en) | 2006-05-10 | 2006-05-10 | Ester exchange method for producing pure glycerin from coarse glycerin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610020997 CN101070269A (en) | 2006-05-10 | 2006-05-10 | Ester exchange method for producing pure glycerin from coarse glycerin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101070269A true CN101070269A (en) | 2007-11-14 |
Family
ID=38897705
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610020997 Pending CN101070269A (en) | 2006-05-10 | 2006-05-10 | Ester exchange method for producing pure glycerin from coarse glycerin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101070269A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267874A (en) * | 2011-06-22 | 2011-12-07 | 南通市康桥油脂有限公司 | Production process for glycerol by virtue of continuous rectification |
| CN101696154B (en) * | 2009-09-23 | 2013-06-05 | 如皋市双马化工有限公司 | Glycerol distilling process and special glycerol distillation tower thereof |
| CN105085171A (en) * | 2015-04-16 | 2015-11-25 | 彭才文 | High purity glycerin refining method by using saponification hydrolysis esterification byproduct |
-
2006
- 2006-05-10 CN CN 200610020997 patent/CN101070269A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696154B (en) * | 2009-09-23 | 2013-06-05 | 如皋市双马化工有限公司 | Glycerol distilling process and special glycerol distillation tower thereof |
| CN102267874A (en) * | 2011-06-22 | 2011-12-07 | 南通市康桥油脂有限公司 | Production process for glycerol by virtue of continuous rectification |
| CN105085171A (en) * | 2015-04-16 | 2015-11-25 | 彭才文 | High purity glycerin refining method by using saponification hydrolysis esterification byproduct |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100567246C (en) | A kind of processing method of producing high-purity L-lactic acid | |
| CN101195572A (en) | Method for synthesizing fatty acid methyl ester | |
| CN103709016A (en) | Process and device for refining glycol dimethyl ether by using pervaporation method | |
| CN1299976C (en) | Method of solvent extraction purification of wet method phosphoric acid produced from medium and low grade phosphosus ore | |
| CN103264998A (en) | Recycle of calcium phosphate | |
| CN102320585A (en) | Method for direct production of industrial-grade ammonium biphosphate by wet-process phosphoric acid | |
| CN101182281A (en) | Method for refining biodiesel byproduct glycerin | |
| CN102675094B (en) | Energy-saving and yield-improving production method of ethyl acetate | |
| CN101070269A (en) | Ester exchange method for producing pure glycerin from coarse glycerin | |
| CN102173991A (en) | Continuous alcohol-removing device and alcohol-removing method of di-sec-octyl phthalate | |
| CN106495174A (en) | Attapulgite wet method bisgallic acid activation method | |
| CN103848739A (en) | Production method of high-purity dimethyl fumarate | |
| CN102041177B (en) | Method for preparing biodiesel | |
| CN201990614U (en) | Continuous dealcoholizing device used for dicapryl phthalate | |
| CN101475444B (en) | Partial dehydration and purification process for crude glycerine | |
| CN103408474A (en) | Efficient production method of high-purity N-acetyl-D, L-methionine | |
| CN108164416B (en) | Novel process for preparing monomethyl azelate based on biodiesel | |
| CN101100435A (en) | Method for preparing L-ornithine-L-aspartate | |
| CN101058527A (en) | Concentration of glycerol | |
| CN1161316C (en) | Lactic acid refining short range distillation process with drum evaporator | |
| CN1884249A (en) | Clean production method for dioctyl phthalate | |
| CN1459441A (en) | Production technique of medical pure glycerin from crude glycerin by ester exchange method | |
| CN100368371C (en) | Method for preparing calcium formate | |
| CN103073579A (en) | Production technology for HEDP with low arsenic content | |
| CN105418378A (en) | Purification technology of ester exchange by-product glycerol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |