CN1459441A - Production technique of medical pure glycerin from crude glycerin by ester exchange method - Google Patents
Production technique of medical pure glycerin from crude glycerin by ester exchange method Download PDFInfo
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- CN1459441A CN1459441A CN 02113774 CN02113774A CN1459441A CN 1459441 A CN1459441 A CN 1459441A CN 02113774 CN02113774 CN 02113774 CN 02113774 A CN02113774 A CN 02113774A CN 1459441 A CN1459441 A CN 1459441A
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- glycerine
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Abstract
A process for preparing medical-pure glycerine from the ester exchange process crude glycerine includes such steps as acidifying by concentrated sulfuric acid, treating with medicament for removing impurities including fatty acid, methyl ester, colloid, pigment, etc., then vacuum concentrating to form crude glycerine, cyclic degassing and drying, cyclic distilling, deodoring and decoloring to obtain the medical-pure glycerine. Its advantage is high purity up to 99.5% or more.
Description
1. technical field
The present invention relates to a kind of production technique of producing medicinal pure glycerin, particularly a kind of production technique of utilizing medical pure glycerin from crude glycerin by ester exchange method.
2. background technology
The content of glycerine is 40～70% in the ester-interchange method raw glycerine, contains a large amount of methyl esters, pigment, colloid and other impurity.With the ester-interchange method raw glycerine is that raw material generally is a manufacture glycerine, and added value of product is low.Utilize the technology of the processed pure glycerin of ion exchange resin, though technical be effectively because the cost issues that resin regeneration and waste resin are handled is not suitable for large-scale commercial production.
The object of the present invention is to provide a kind of production technique of utilizing existing installation, the simple ester-interchange method raw glycerine of technology to produce medicinal pure glycerin.
3. summary of the invention
The object of the present invention is achieved like this, a kind of production technique of medical pure glycerin from crude glycerin by ester exchange method, and the ester-interchange method raw glycerine is removed free fatty acids, methyl esters, colloid, pigment, SO through chemicals treatment
4 2-With impurity such as heavy metal ion, vacuum concentration becomes raw glycerine then, raw glycerine obtains medicinal pure glycerin through circulating degasification drying, circulation distillation, deodorizing, bleaching process, it is characterized in that: with the ester-interchange method raw glycerine before chemicals treatment, earlier with the vitriol oil acidifying of ester-interchange method raw glycerine, its pH is 5～6.5, and acidificatoin time is between 1 hour to 1 and a half hours, and temperature is controlled at 80～90 ℃.
Described chemicals treatment, with acidified ester-interchange method raw glycerine be put into retort 1. in, be heated to 95～100 ℃, add 1.5%～3.5% the calcium oxide account for raw materials quality or calcium hydroxide to remove free fatty acids and most of SO
4 2-, impurity such as precipitation absorption that utilization generates and sedimentation methyl esters, colloid, pigment; With the material after handling with the pressure filter circulating filtration deliver to retort 2. in, be heated to 95～100 ℃, adding accounts for 1%～2% hydrated barta of raw materials quality and removes SO
4 2-, utilize the barium sulfate precipitate adsorpting pigment; Add oxalic acid or solubility oxalate and flocculating aids such as diatomite etc. again and remove calcium, barium ion and other heavy metal ion.
Vacuum concentration divides two sections to carry out, and first section raw glycerine boiling temperature is controlled at 85～105 ℃, and vacuum is 90kpa; Second section raw glycerine boiling temperature is controlled at 65～70 ℃, and vacuum is 10kpa, and the concentration of handling the back raw glycerine like this is 88～93%.
Compare with prior art, the present invention can effectively remove methyl esters a large amount of in the ester-interchange method raw glycerine, pigment, colloid and other impurity, the purity that improves glycerol product reaches more than 99.5%, finished product glycerine can reach national medicinal glycerin standard and American-European standards of pharmacopoeia, lipid acid and ester, SO in the finished product glycerine
4 2-, the content of heavy metal ion and arsenic is lower than American-European standard; Add oxalic acid among the present invention and can remove calcium, barium ion and other heavy metal ion, and can reduce the basicity of raw glycerine, the generation of side reaction when reducing glycerol distillation adopts calcium oxide or calcium hydroxide and hydrated barta and oxalic acid that raw glycerine is handled and can effectively be reduced production costs.
4. description of drawings
Fig. 1 is the process flow sheet of the embodiment of the invention.
5. embodiment
As shown in Figure 1, a kind of ester-interchange method raw glycerine is produced the production technique of medicinal pure glycerin, and earlier with the vitriol oil acidifying of ester-interchange method raw glycerine, its pH is 6, and acidificatoin time is 1 hour 10 minutes, and temperature is controlled at 85 ℃.
Acidified ester-interchange method raw glycerine is carried out chemicals treatment, with acidifying ester-interchange method raw glycerine be put into retort 1. in, be heated to 98 ℃, add the calcium oxide account for raw materials quality 2.5% or calcium hydroxide to remove free fatty acids and most of SO
4 2-, utilize the precipitation absorption of its generation and sedimentation methyl esters, colloid, pigment etc.; With the material after handling by the pressure filter circulating filtration deliver to retort 2. in, be heated to 98 ℃, add and account for raw materials quality 1.2% hydrated barta reagent and remove SO
4 2-, utilize the barium sulfate precipitate adsorpting pigment, add oxalic acid or solubility oxalate and flocculating aids such as diatomite again, remove calcium, barium ion and other heavy metal ion, deliver in the storage tank with pressure filter again.
Raw glycerine after the chemicals treatment is carried out vacuum concentration, and vacuum concentration divides two sections to carry out, and first section raw glycerine boiling temperature is controlled at 100 ℃, and vacuum is 90kpa; Second section raw glycerine boiling temperature is controlled at 68 ℃, and vacuum is 10kpa, and the concentration of handling the back raw glycerine like this is 88～93%, and the glycerine after handling is delivered to storage tank.
Glycerine behind the vacuum concentration is sloughed moisture and other byproduct by the circulating degasification drying tower, and with the glycerine drying.
It is still kettle that the circulation water distilling apparatus is injected in the heating of anhydrous glycerol heater via after the drying treatment, the residue of still kettle bottom is deviate from continuously by scrapper thin film evaporator, scraper plate book film evaporator is sent into the glycerine that reclaims in the circulating degasification drying tower, residue is collected got rid of.
The deodorizing tower deodorizing is sent in the glycerine that distills out condensation under 120 ℃ of temperature then, just obtains medicinal pure glycerin through the bleacher decolouring again.
Adopt the index of the medicinal pure glycerin that obtains of the present invention as follows:
Glycerol content is 99.73%, and colourity (hazen) is 5, muriate (CL%)＜0.0015, vitriol (SO
4 2-%)＜0.002, acidity or alkalinity (mol/100g)＜0.0018, saponification equivalent (mol/100g)＜0.08, arsenic content (mg/kg)＜2, heavy metal content (mg/kg)＜2, lipid acid that contains in the 40g pure glycerin sample and ester class consume 0.1mol/1NaOH0.45ml.
Claims (3)
1. the production technique of a medical pure glycerin from crude glycerin by ester exchange method, the ester-interchange method raw glycerine is removed free fatty acids, methyl esters, colloid, pigment, SO through chemicals treatment
4 2-With impurity such as heavy metal ion, vacuum concentration becomes raw glycerine then, raw glycerine obtains medicinal pure glycerin through circulating degasification drying, circulation distillation, deodorizing, bleaching process, it is characterized in that: with the ester-interchange method raw glycerine before chemicals treatment, earlier with the vitriol oil acidifying of ester-interchange method raw glycerine, its pH is 5～6.5, and acidificatoin time is between 1 hour to 1 and a half hours, and temperature is controlled at 80～90 ℃.
2. the production technique of medical pure glycerin from crude glycerin by ester exchange method as claimed in claim 1, it is characterized in that: described chemicals treatment, with acidified ester-interchange method raw glycerine be put into retort 1. in, be heated to 95～100 ℃, add 1.5%～3.5% calcium oxide or the calcium hydroxide account for raw materials quality and remove free fatty acids and most of SO
4 2-, impurity such as precipitation absorption that utilization generates and sedimentation methyl esters, colloid, pigment; With the material after handling with the pressure filter circulating filtration deliver to retort 2. in, be heated to 95～100 ℃, adding accounts for 1%～2% hydrated barta of raw materials quality and removes SO
4 2-, utilize the barium sulfate precipitate adsorpting pigment, add oxalic acid or solubility oxalate and flocculating aids such as diatomite etc. again and remove calcium, barium ion and other heavy metal ion.
3. the production technique of medical pure glycerin from crude glycerin by ester exchange method as claimed in claim 1 or 2, it is characterized in that: vacuum concentration divides two sections to carry out, and first section raw glycerine boiling temperature is controlled at 85～105 ℃, and vacuum is 90kpa; Second section raw glycerine boiling temperature is controlled at 65～70 ℃, and vacuum is 10kpa, and the concentration of handling the back raw glycerine like this is 88～93%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02113774 CN1459441A (en) | 2002-05-24 | 2002-05-24 | Production technique of medical pure glycerin from crude glycerin by ester exchange method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02113774 CN1459441A (en) | 2002-05-24 | 2002-05-24 | Production technique of medical pure glycerin from crude glycerin by ester exchange method |
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| CN1459441A true CN1459441A (en) | 2003-12-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 02113774 Pending CN1459441A (en) | 2002-05-24 | 2002-05-24 | Production technique of medical pure glycerin from crude glycerin by ester exchange method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010136838A1 (en) * | 2009-05-29 | 2010-12-02 | The Gtbe Company Nv | Method for processing crude glycerol waste streams |
| CN102417439A (en) * | 2011-10-24 | 2012-04-18 | 南通市康桥油脂有限公司 | Processing technology for glycerin aqueous solution produced from grease hydrolysis |
| CN101759526B (en) * | 2010-01-13 | 2012-07-18 | 湖南省林业科学院 | Refining production method of glycerin |
| GB2463300B (en) * | 2008-09-05 | 2012-12-05 | Wei Ming Chang | Glycerol (medical grade) preparation method using a by-product of a bio-diesel process |
| CN104707353A (en) * | 2015-02-12 | 2015-06-17 | 浙江华诺化工有限公司 | Glycerin distillation system |
-
2002
- 2002-05-24 CN CN 02113774 patent/CN1459441A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2463300B (en) * | 2008-09-05 | 2012-12-05 | Wei Ming Chang | Glycerol (medical grade) preparation method using a by-product of a bio-diesel process |
| WO2010136838A1 (en) * | 2009-05-29 | 2010-12-02 | The Gtbe Company Nv | Method for processing crude glycerol waste streams |
| CN101759526B (en) * | 2010-01-13 | 2012-07-18 | 湖南省林业科学院 | Refining production method of glycerin |
| CN102417439A (en) * | 2011-10-24 | 2012-04-18 | 南通市康桥油脂有限公司 | Processing technology for glycerin aqueous solution produced from grease hydrolysis |
| CN104707353A (en) * | 2015-02-12 | 2015-06-17 | 浙江华诺化工有限公司 | Glycerin distillation system |
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