CN103664523A - Method for refining biodiesel by-product crude glycerine - Google Patents
Method for refining biodiesel by-product crude glycerine Download PDFInfo
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- CN103664523A CN103664523A CN201210316073.2A CN201210316073A CN103664523A CN 103664523 A CN103664523 A CN 103664523A CN 201210316073 A CN201210316073 A CN 201210316073A CN 103664523 A CN103664523 A CN 103664523A
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- solution
- glycerine
- crude glycerine
- subnatant
- diesel oil
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for refining biodiesel by-product crude glycerine. The method comprises the following steps: saponifying, namely weighing a certain amount of biodiesel by-product crude glycerine, and carrying out saponification according to the molar ratio of potassium hydroxide methanol solution to esters being 1-2; 2, acidizing, namely adding 30g of saponified crude glycerine to a 500mL of three-necked flask, adding a polar reagent methanol as an extracting agent according to the volume ratio of 4:1 to 1:4, adding a dilute acid solution to adjust the pH of the solution to be 1-5, agitating, standing and layering and collecting subnatant; 3, adsorbing, namely respectively adding 50-80mg/L of activated carbon to the subnatant, heating at 70 DEG C to remove methanol, finally pouring the solution into a separating funnel, cooling and layering: 4, determining the content of glycerine. The method has the beneficial effects that the biodiesel by-product crude glycerine is refined, so that not only is the value of crude glycerine improved, but also raw materials are supplied to the fields such as pharmacy, food and the like. The method disclosed by the invention is simple, mild in reaction condition, low in requirement on equipment, and strong in practicability.
Description
Technical field
The present invention relates to chemical field, specifically a kind of method of biological diesel oil byproduct refining crude glycerin.
Background technology
Pure glycerine (glycerol) is a kind of colourless pleasantly sweet glutinous thick liquid, is widely used in pharmacy, food, makeup, glassine paper, insulating material and chemical industry.The animal-plant oil of take produces a large amount of by product raw glycerines in raw material production biofuel process, the salts contg that raw glycerine can be removed in glycerine through large porous strong acid ion exchange resin is purified, and the purification of most glycerine is all by first glycerine being distilled mutually and removes impurity with membrane filtration.But these ways are high to equipment requirements, and power consumption is large.
Summary of the invention
According to above-mentioned weak point, the object of this invention is to provide a kind of method of biological diesel oil byproduct refining crude glycerin.
Technical scheme of the present invention is: a kind of method of biological diesel oil byproduct refining crude glycerin, it includes
1, saponification: take the biological diesel oil byproduct raw glycerine of certain mass, carry out saponification reaction by potassium hydroxide methanol solution and ester class mol ratio 1-2;
2, acidifying: add 30g through the raw glycerine of saponification in 500mL there-necked flask, by volume for 4:1-l:4 adds polar reagent methanol as extractant, then add dilute acid soln, the pH that makes solution is l～5, stirs, and stratification is got subnatant;
3, absorption: the gac toward adding respectively 50-80mg/L in subnatant adds heat abstraction methyl alcohol at 70 ℃; Finally by the solution separating funnel of falling people, cooling layering;
4, measure glycerol content.
Preferably: described dilute acid soln is sulfuric acid, phosphoric acid or acetic acid solution.
The invention has the beneficial effects as follows: by the present invention, the byproduct raw glycerine of biofuel is refined, not only improved the value of raw glycerine, more the field such as pharmacy, food provides raw material, the inventive method is simple, reaction conditions is gentle, not high to equipment requirements, can be practical.
Embodiment
According to specific embodiment, the present invention will be further described below.
A method for biological diesel oil byproduct refining crude glycerin, it includes: 1, saponification: take the biological diesel oil byproduct raw glycerine of certain mass, by potassium hydroxide methanol solution and ester class mol ratio 2, carry out saponification reaction; 2, acidifying: add 30g through the raw glycerine of saponification in 500mL there-necked flask, by volume for 1:4 adds polar reagent methanol as extractant, then add dilution heat of sulfuric acid, the pH that makes solution is 2, stirs, and stratification is got subnatant; 3, absorption: the gac toward adding respectively 50mg/L in subnatant adds heat abstraction methyl alcohol at 70 ℃; Finally by the solution separating funnel of falling people, cooling layering; 4, measuring glycerol content is 73.56%.
Embodiment 2
A method for biological diesel oil byproduct refining crude glycerin, it includes: 1, saponification: take the biological diesel oil byproduct raw glycerine of certain mass, by potassium hydroxide methanol solution and ester class mol ratio 2, carry out saponification reaction; 2, acidifying: add 30g through the raw glycerine of saponification in 500mL there-necked flask, by volume for 4:1 adds polar reagent methanol as extractant, then add dilution heat of sulfuric acid, the pH that makes solution is 5, stirs, and stratification is got subnatant; 3, absorption: the gac toward adding respectively 80mg/L in subnatant adds heat abstraction methyl alcohol at 70 ℃; Finally by the solution separating funnel of falling people, cooling layering; 4, measuring glycerol content is 79.17%.
Embodiment 3
A method for biological diesel oil byproduct refining crude glycerin, it includes 1, saponification: take the biological diesel oil byproduct raw glycerine of certain mass, by potassium hydroxide methanol solution and ester class mol ratio 1.5, carry out saponification reaction; 2, acidifying: add 30g through the raw glycerine of saponification in 500mL there-necked flask, by volume for 2:1 adds polar reagent methanol as extractant, then add dilution heat of sulfuric acid, the pH that makes solution is 24, stirs, and stratification is got subnatant; 3, absorption: the gac toward adding respectively 60mg/L in subnatant adds heat abstraction methyl alcohol at 70 ℃; Finally by the solution separating funnel of falling people, cooling layering; 4, measuring glycerol content is 86.34%.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, those of ordinary skills are to be understood that, technical scheme of the present invention is modified or is equal to replacement, and do not depart from aim and the scope of technical solution of the present invention, within it is all encompassed in claim scope of the present invention.
Claims (2)
1. a method for biological diesel oil byproduct refining crude glycerin, is characterized in that: it includes
1) saponification: take the biological diesel oil byproduct raw glycerine of certain mass, carry out saponification reaction by potassium hydroxide methanol solution and ester class mol ratio 1-2;
2) acidifying: add 30g through the raw glycerine of saponification in 500mL there-necked flask, by volume for 4:1-l:4 adds polar reagent methanol as extractant, then add dilute acid soln, the pH that makes solution is l～5, stirs, and stratification is got subnatant;
3) absorption: the gac toward adding respectively 50-80mg/L in subnatant adds heat abstraction methyl alcohol at 70 ℃; Finally by the solution separating funnel of falling people, cooling layering;
4) measure glycerol content.
2. according to the method for a kind of biological diesel oil byproduct refining crude glycerin claimed in claim 1, it is characterized in that: described dilute acid soln is sulfuric acid, phosphoric acid or acetic acid solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210316073.2A CN103664523A (en) | 2012-08-31 | 2012-08-31 | Method for refining biodiesel by-product crude glycerine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210316073.2A CN103664523A (en) | 2012-08-31 | 2012-08-31 | Method for refining biodiesel by-product crude glycerine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103664523A true CN103664523A (en) | 2014-03-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210316073.2A Pending CN103664523A (en) | 2012-08-31 | 2012-08-31 | Method for refining biodiesel by-product crude glycerine |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585424A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Removal method of organic chlorine in by-product glycerol of transesterification reaction of grease |
| CN106831343A (en) * | 2015-12-03 | 2017-06-13 | 浙江医药股份有限公司新昌制药厂 | A kind of isolation and purification method of grease ester bond byproduct of reaction |
| GB2549139A (en) * | 2016-04-07 | 2017-10-11 | A & C Freeman | Glycerol from biodiesel waste |
| CN111871364A (en) * | 2020-07-24 | 2020-11-03 | 武汉轻工大学 | Preparation method of solid acid and method for purifying glycerin from biodiesel byproduct |
| CN115404129A (en) * | 2022-09-16 | 2022-11-29 | 临沂明英工贸有限公司 | Production process for producing acidified oil from mixed oil leftover material |
| CN115612553A (en) * | 2022-10-31 | 2023-01-17 | 上海中器环保科技有限公司 | Process for recovering biodiesel from crude glycerol |
-
2012
- 2012-08-31 CN CN201210316073.2A patent/CN103664523A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585424A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Removal method of organic chlorine in by-product glycerol of transesterification reaction of grease |
| CN106831343A (en) * | 2015-12-03 | 2017-06-13 | 浙江医药股份有限公司新昌制药厂 | A kind of isolation and purification method of grease ester bond byproduct of reaction |
| CN106831343B (en) * | 2015-12-03 | 2020-10-20 | 浙江医药股份有限公司新昌制药厂 | Separation and purification method of grease ester bond reaction by-product |
| GB2549139A (en) * | 2016-04-07 | 2017-10-11 | A & C Freeman | Glycerol from biodiesel waste |
| GB2549139B (en) * | 2016-04-07 | 2019-01-30 | A & C Freeman | Process for recovery of glycerol from biodiesel production streams |
| CN111871364A (en) * | 2020-07-24 | 2020-11-03 | 武汉轻工大学 | Preparation method of solid acid and method for purifying glycerin from biodiesel byproduct |
| CN115404129A (en) * | 2022-09-16 | 2022-11-29 | 临沂明英工贸有限公司 | Production process for producing acidified oil from mixed oil leftover material |
| CN115612553A (en) * | 2022-10-31 | 2023-01-17 | 上海中器环保科技有限公司 | Process for recovering biodiesel from crude glycerol |
| CN115612553B (en) * | 2022-10-31 | 2024-04-05 | 上海中器环保科技有限公司 | Process for recovering biodiesel from crude glycerol |
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Application publication date: 20140326 |