CN112159728A - Method for reducing acid value of waste oil by esterification - Google Patents
Method for reducing acid value of waste oil by esterification Download PDFInfo
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- CN112159728A CN112159728A CN202010943116.4A CN202010943116A CN112159728A CN 112159728 A CN112159728 A CN 112159728A CN 202010943116 A CN202010943116 A CN 202010943116A CN 112159728 A CN112159728 A CN 112159728A
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- 238000005886 esterification reaction Methods 0.000 title claims abstract description 181
- 230000032050 esterification Effects 0.000 title claims abstract description 115
- 239000002699 waste material Substances 0.000 title claims abstract description 63
- 239000002253 acid Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 29
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 129
- 239000000243 solution Substances 0.000 claims abstract description 56
- 239000011259 mixed solution Substances 0.000 claims abstract description 36
- 239000004519 grease Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000011541 reaction mixture Substances 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 abstract description 44
- 239000003921 oil Substances 0.000 description 45
- 235000019198 oils Nutrition 0.000 description 45
- 239000007788 liquid Substances 0.000 description 15
- 239000010806 kitchen waste Substances 0.000 description 12
- 239000003225 biodiesel Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000003208 petroleum Substances 0.000 description 4
- 230000036632 reaction speed Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008162 cooking oil Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/06—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with glycerol
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Lubricants (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for reducing acid value of waste grease by esterification. The method comprises the following steps: mixing waste oil and glycerol: uniformly mixing the waste grease and glycerol to obtain a mixed solution, then heating the mixed solution to 120-135 ℃, then heating to 160-175 ℃, and finally heating to 195-205 ℃; a first esterification reaction: carrying out esterification reaction on the heated mixed solution at the residual vacuum pressure of 6000-9000Pa and the temperature of 200-215 ℃ to obtain a first esterification solution; second esterification reaction: carrying out esterification reaction on the first esterification solution at the vacuum residual pressure of 6000-9000Pa and the temperature of 210-220 ℃ to obtain a second esterification solution; the temperature of the second esterification reaction is higher than the temperature of the first esterification reaction. The method can reduce the acid value of the waste oil through a small amount of glycerin at a lower temperature.
Description
Technical Field
The invention relates to the field of grease chemical biodiesel, in particular to a method for reducing acid value of waste grease by esterification.
Background
The preparation of biodiesel from vegetable oil has attracted people's attention especially, and because the combustibility of the biodiesel is not inferior to that of petroleum diesel, the biodiesel can be directly used in the field of petroleum diesel such as diesel engines, and people generally think that the biodiesel is a substitute for the petroleum diesel in the future. The biodiesel has the advantages of no toxicity, biodegradability, high cetane number, less emission of sulfide carbon monoxide, and greatly reduced emission of carbon dioxide compared with petroleum diesel because the carbon emitted by the biodiesel is from the atmosphere.
At present, because of the shortage of vegetable fat in China, the biodiesel production mainly takes high-acid-value kitchen waste fat and hogwash oil as waste fat as raw materials. The production technology of waste grease biodiesel is emerging, various technical methods are infinite, and the problems of low efficiency and large energy consumption exist in the prior art through glycerol esterification of waste grease.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to realize the acid value reduction of the waste oil at a lower temperature by a small amount of glycerin.
In order to solve the technical problem, the invention provides a method for reducing the acid value of waste oil by esterification.
The invention provides a method for reducing acid value of waste grease by esterification, which comprises the following steps:
mixing waste oil and glycerol: uniformly mixing the waste grease and glycerol to obtain a mixed solution, then heating the mixed solution to 120-135 ℃, then heating to 160-175 ℃, and finally heating to 195-205 ℃;
a first esterification reaction: carrying out esterification reaction on the heated mixed solution at the residual vacuum pressure of 6000-9000Pa and the temperature of 200-215 ℃ to obtain a first esterification solution;
second esterification reaction: carrying out esterification reaction on the first esterification solution at the vacuum residual pressure of 6000-9000Pa and the temperature of 210-220 ℃ to obtain a second esterification solution; the temperature of the second esterification reaction is higher than the temperature of the first esterification reaction.
Further, the adding mass of the glycerol is 5-20% of the mass of the waste grease.
Furthermore, the acid value of the waste oil is 20-150 mgKOH/g.
Further, the reaction mixture after temperature rise is subjected to esterification reaction for 2-4 hours at the vacuum residual pressure of 6000-9000Pa and the temperature of 200-215 ℃ to obtain a first esterification solution.
Further, the first esterification liquid is subjected to esterification reaction for 2-4 hours at the vacuum residual pressure of 6000-9000Pa and the temperature of 210-220 ℃ to obtain a second esterification liquid.
Further, the reaction mixed solution after temperature rise is subjected to esterification loop reaction at the vacuum residual pressure of 6000-9000Pa and the temperature of 200-215 ℃ to obtain a first esterification solution.
Further, the first esterification liquid is subjected to esterification loop reaction at the vacuum residual pressure of 6000-9000Pa and the temperature of 210-220 ℃ to obtain a second esterification liquid.
Further, the reaction mixed solution after temperature rise is subjected to esterification reaction at vacuum residual pressure of 8000-9000Pa and temperature of 200-210 ℃ to obtain the first esterification solution.
Further, the first esterification liquid is subjected to esterification reaction at vacuum residual pressure of 8000-9000Pa and temperature of 210-215 ℃ to obtain a second esterification liquid.
Further, the temperature of the mixed solution is first raised to 135 ℃ at 120 ℃ by the U-shaped heat exchange reactor, then raised to 175 ℃ at 160 ℃ and finally raised to 205 ℃ at 195 ℃.
Compared with the prior art, the invention has the advantages that: uniformly mixing the waste oil and glycerol to obtain a mixed solution, then heating the mixed solution to the temperature of 120-; in order to reduce the loss of glycerin, the glycerin esterification temperature is as low as possible, but the low temperature affects the reaction speed and efficiency, in order to keep the esterification reaction speed, the first esterification reaction temperature is controlled to be carried out under the vacuum residual pressure of 6000-minus 9000Pa and the temperature of 200-minus 215 ℃, the esterification reaction temperature is low, the loss of the glycerol polymerization is reduced, then the second esterification reaction is carried out under the vacuum residual pressure of 6000-minus 9000Pa and the temperature of 200-minus 215 ℃, the glycerol content after the first-stage esterification reaction is reduced, the temperature is increased to 200-minus 215 ℃, the reaction speed can be further ensured, and the loss of the glycerol polymerization is reduced, therefore, the acid value of the waste oil can be reduced by a small amount of glycerin at a lower temperature, the acid value of the finally obtained second esterification liquid can be below 1.5mgKOH/g, and the lowest acid value can be as low as 0.62 mgKOH/g.
Drawings
The features and advantages of the present invention will be more clearly understood by reference to the accompanying drawings, which are illustrative and not to be construed as limiting the invention in any way, and in which:
fig. 1 is a schematic structural diagram of a waste grease esterification system according to the present invention.
Description of reference numerals: 01. an esterification oil tank; 02. a glycerin tank; 03. a waste grease tank; 04. A U-shaped heat exchanger; 05. a first esterification reaction tower; 06. a second esterification reaction tower; 07. a balance condenser; 08. a first water pump; 09. a steady flow variable frequency screw pump; 10. a steady flow variable frequency gear pump; 11. a first circulation pump; 12. a feed pump; 13. a second circulation pump; 14. an esterification liquid extraction pump; 15. and a second water pump.
Detailed Description
The specific embodiment provides a method for reducing acid value of waste grease by esterification, which comprises the following steps:
1) mixing waste oil and glycerol: uniformly mixing the waste grease and glycerol to obtain a mixed solution, then heating the mixed solution to 120-135 ℃, then to 160-175 ℃ and finally to 195-205 ℃ through a U-shaped heat exchange reactor; the adding mass of the glycerol is 5-20% of the mass of the waste grease; the acid value of the waste oil is 20-150 mgKOH/g;
2) a first esterification reaction: carrying out esterification loop reaction on the heated mixed solution at the residual vacuum pressure of 6000-9000Pa and the temperature of 200-215 ℃ for 2-4 hours to obtain a first esterification solution;
in a preferred embodiment, the mixed solution after temperature rise is subjected to esterification loop reaction for 2-4 hours at vacuum residual pressure of 8000-9000Pa and temperature of 200-210 ℃ to obtain a first esterification solution;
3) second esterification reaction: carrying out esterification loop reaction on the first esterification solution at the vacuum residual pressure of 6000-9000Pa and the temperature of 210-220 ℃ for 2-4 hours to obtain a second esterification solution; the temperature of the second esterification reaction is higher than the temperature of the first esterification reaction.
In a preferred embodiment, the first esterification solution is subjected to esterification loop reaction for 2-4 hours at vacuum residual pressure of 8000-9000Pa and temperature of 210-215 ℃ to obtain a second esterification solution.
It should be noted that the waste grease in this embodiment includes one or more of swill oil, kitchen waste grease, waste cooking oil, and rancid oil.
With reference to fig. 1, the method provided by the present embodiment is implemented by a waste grease esterification system, which is sequentially connected to a glycerin tank 02, a U-shaped heat exchanger 04, a first esterification reaction tower 05, and a second esterification reaction tower 6; in addition, the waste grease tank 03 is communicated with the U-shaped heat exchanger 04, the esterification oil tank 01 is communicated with the U-shaped heat exchanger 04, and the equilibrium condenser 07 is respectively communicated with the first esterification reaction tower 05 and the second esterification reaction tower 6; further, the glycerin tank 02 is communicated with the U-shaped heat exchanger 04 through a steady-flow variable-frequency screw pump 09, the waste grease tank 03 is communicated with the U-shaped heat exchanger 04 through a steady-flow variable-frequency gear pump 10, a discharge port at the bottom of the first esterification reaction tower 05 is communicated with a feed port of the first circulating pump 11, a discharge port of the first circulating pump 11 is communicated with a feed port at the side of the first esterification reaction tower 05, and a discharge port of the U-shaped heat exchanger 04 is communicated with a feed port of the first circulating pump 11; further, a discharge port at the bottom of the second esterification reaction tower 6 is communicated with a feed port of a second circulating pump 13, a discharge port of the second circulating pump 13 is communicated with a feed port at the side surface of the second esterification reaction tower 6, and the first esterification reaction tower 05 is communicated with the second esterification reaction tower 6 through a feed pump 12; the feed inlet of the balance condenser 07 is communicated with a first water pump 08, the discharge outlet is connected with a second water pump 15, and the water pump introduces and discharges the water of the balance condenser 07 to realize the circulation of cooling water.
Further, the discharge port of the second esterification reaction tower 6 is connected with the U-shaped heat exchanger 04 through an esterification liquid extraction pump 14, the temperature of the kitchen waste oil is increased through heat exchange of the esterification liquid and the fed waste oil, and the esterification liquid is reduced to a reasonable level.
The working process of the system is as follows:
opening a high-acid-value waste grease delivery pipe valve, conveying reasonable flow of waste grease in a waste grease tank by using a steady-flow variable-frequency gear pump, opening a glycerin quantity delivery pipe valve corresponding to the acid value, conveying reasonable flow of glycerin in the glycerin tank by using a steady-flow variable-frequency screw pump, mixing two-phase fluid by using a Kenikos static mixer before entering a U-shaped heat exchanger, performing three-stage heat exchange with esterified oil in the U-shaped heat exchanger, introducing the heat-exchange high-acid-value waste grease and glycerin mixed oil into a primary esterification reaction tower, starting a first esterification pump, starting a heat-conducting oil constant-temperature circulating system arranged in the first esterification reaction tower, starting a balance condenser, performing a first loop circulating esterification reaction, gradually raising the esterification liquid level along with deep esterification, reaching an esterification liquid overflow port at the top of the tower after 3 hours, sampling to detect the acid value, and determining that the acid value is less than 3.5 as qualified, introducing the first esterification, and (3) starting a second circulating esterification pump, starting a jacket heat-conducting oil constant-temperature circulating system in a second esterification reaction tower, (wherein a vacuum pump, a balance condenser and the first-stage esterification share) to perform second loop circulating esterification reaction, gradually raising the esterification liquid level along with the deep esterification, reaching an esterification liquid overflow port at the top of the tower after 3 hours, sampling and detecting the acid value, and determining that the acid value is less than 1.5. (if the acid value does not reach the standard, the flow of the glycerol is adjusted in time) the qualified esterified oil is exchanged with the fed waste oil and then sent to the ester exchange process.
The preferred embodiments of the present invention are described in detail below.
Example 1
A method for reducing acid value of waste oil by esterification comprises the following steps:
1) mixing the kitchen waste grease with glycerol: uniformly mixing waste oil and glycerol to obtain a mixed solution, heating the mixed solution to 120 ℃ through a three-stage U-shaped heat exchange reactor, then heating to 175 ℃, and finally heating to 195 ℃; the adding mass of the glycerol is 18% of the mass of the waste oil; the acid value of the waste oil is 144 mgKOH/g;
2) a first esterification reaction: carrying out esterification loop reaction on the heated reaction mixed solution for 3 hours at the vacuum residual pressure of 8000Pa and the temperature of 200 ℃ to obtain a first esterification solution; detecting that the acid value of the first esterification solution is 1.5 mgKOH/g;
3) second esterification reaction: carrying out esterification loop reaction on the first esterification solution for 3 hours at vacuum residual pressure of 8000Pa and temperature of 208.4 ℃ to obtain a second esterification solution; the acid value of the second esterification solution was measured to be 0.62 mgKOH/g.
Example 2
A method for reducing acid value of waste oil by esterification comprises the following steps:
1) mixing the kitchen waste grease with glycerol: uniformly mixing kitchen waste oil and glycerol to obtain a mixed solution, and then heating the mixed solution to 135 ℃, 160 ℃ and 205 ℃ through a three-stage U-shaped heat exchange reactor; the adding mass of the glycerol is 18% of the mass of the waste oil; the acid value of the waste oil is 144 mgKOH/g;
2) a first esterification reaction: carrying out esterification loop reaction on the heated reaction mixed solution for 4 hours at the residual vacuum pressure of 7000Pa and the temperature of 205 ℃ to obtain a first esterification solution; detecting that the acid value of the first esterification solution is 4.5 mgKOH/g;
3) second esterification reaction: carrying out esterification loop reaction on the first esterification solution at the residual vacuum pressure of 7000Pa and the temperature of 215 ℃ for 4 hours to obtain a second esterification solution; the acid value of the second esterification solution was measured to be 1.2 mgKOH/g.
Example 3
A method for reducing acid value of waste oil by esterification comprises the following steps:
1) mixing the kitchen waste grease with glycerol: uniformly mixing kitchen waste oil and glycerol to obtain a mixed solution, and then heating the mixed solution to 130 ℃, 170 ℃ and 200 ℃ through a three-stage U-shaped heat exchange reactor; the adding mass of the glycerol is 5% of the mass of the waste oil; the acid value of the waste oil is 30 mgKOH/g;
2) a first esterification reaction: carrying out esterification loop reaction on the heated reaction mixed solution for 2 hours at the residual vacuum pressure of 6000Pa and the temperature of 210 ℃ to obtain a first esterification solution; detecting that the acid value of the first esterification solution is 1.8 mgKOH/g;
3) second esterification reaction: carrying out esterification loop reaction on the first esterification solution at the residual vacuum pressure of 6000Pa and the temperature of 220 ℃ for 2 hours to obtain a second esterification solution; the acid value of the second esterification solution was measured to be 0.9 mgKOH/g.
Example 4
A method for reducing acid value of waste oil by esterification comprises the following steps:
1) mixing the kitchen waste grease with glycerol: uniformly mixing kitchen waste oil and glycerol to obtain a mixed solution, and then heating the mixed solution to 130 ℃, 165 ℃ and 200 ℃ through a three-stage U-shaped heat exchange reactor; the adding mass of the glycerol is 20% of the mass of the waste oil; the acid value of the waste oil is 150 mgKOH/g;
2) a first esterification reaction: carrying out esterification loop reaction on the heated mixed solution for 2 hours at vacuum residual pressure of 9000Pa and temperature of 205 ℃ to obtain a first esterification solution; detecting that the acid value of the first esterification solution is 2.5 mgKOH/g;
3) second esterification reaction: carrying out esterification loop reaction on the first esterification solution at vacuum residual pressure of 9000Pa and temperature of 210 ℃ for 2 hours to obtain a second esterification solution; the acid value of the second esterification solution was measured to be 1.1 mgKOH/g.
Example 5
The embodiment provides a method for reducing acid value of waste grease by esterification, which comprises the following steps:
1) mixing the kitchen waste grease with glycerol: uniformly mixing waste oil and glycerol to obtain a mixed solution, heating the mixed solution to 135 ℃, then to 175 ℃ and finally to 195 ℃ through a three-stage U-shaped heat exchange reactor; the adding mass of the glycerol is 10% of the mass of the waste oil; the acid value of the waste oil is 90 mgKOH/g;
2) a first esterification reaction: carrying out esterification loop reaction on the heated mixed solution for 3 hours at the residual vacuum pressure of 7000Pa and the temperature of 200 ℃ to obtain a first esterification solution; detecting that the acid value of the first esterification solution is 1.2 mgKOH/g;
3) second esterification reaction: carrying out esterification loop reaction on the first esterification solution at the residual vacuum pressure of 7000Pa and the temperature of 215 ℃ for 4 hours to obtain a second esterification solution; the acid value of the second esterification solution was measured to be 0.8 mgKOH/g.
Comparative example 1
A method for reducing acid value of waste oil by esterification comprises the following steps:
1) mixing the kitchen waste grease with glycerol: uniformly mixing waste oil and glycerol to obtain a mixed solution, and then heating the mixed solution to 195 ℃ by a heater; the adding mass of the glycerol is 18% of the mass of the waste oil; the acid value of the waste oil is 144 mgKOH/g;
2) a first esterification reaction: carrying out esterification reaction on the heated reaction mixed solution at the temperature of 200 ℃ for 3 hours to obtain a first esterification solution; detecting that the acid value of the first esterification solution is 40 mgKOH/g; and (4) continuing the esterification reaction for 4 hours to obtain a second esterification solution, and detecting that the acid value of the second esterification solution is 15.8 mgKOH/g.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (10)
1. A method for reducing acid value of waste oil by esterification is characterized by comprising the following steps:
mixing waste oil and glycerol: uniformly mixing the waste grease and glycerol to obtain a mixed solution, then heating the mixed solution to 120-135 ℃, then heating to 160-175 ℃, and finally heating to 195-205 ℃;
a first esterification reaction: carrying out esterification reaction on the heated reaction mixed solution at the vacuum residual pressure of 6000-9000Pa and the temperature of 200-215 ℃ to obtain a first esterification solution;
second esterification reaction: carrying out esterification reaction on the first esterification solution at the vacuum residual pressure of 6000-9000Pa and the temperature of 210-220 ℃ to obtain a second esterification solution; the temperature of the second esterification reaction is higher than the temperature of the first esterification reaction.
2. The method according to claim 1, wherein the glycerol is added in an amount of 5-20% by mass based on the mass of the waste oil.
3. The method according to claim 1, wherein the acid value of the waste oil and fat is 20 to 150 mgKOH/g.
4. The method as claimed in claim 1, wherein the temperature of the reaction mixture after temperature rise is increased to 9000Pa under a residual vacuum pressure of 6000 and 215 ℃ for esterification reaction for 2-4 hours to obtain the first esterification solution.
5. The method as claimed in claim 1, wherein the first esterification solution is subjected to esterification reaction at a residual vacuum pressure of 6000-9000Pa and a temperature of 210-220 ℃ for 2-4 hours to obtain the second esterification solution.
6. The method as claimed in claim 1, wherein the heated reaction mixture is subjected to esterification loop reaction at a residual vacuum pressure of 6000-9000Pa and a temperature of 200-215 ℃ to obtain the first esterification solution.
7. The method as claimed in claim 1, wherein the first esterification solution is subjected to esterification loop reaction at a residual vacuum pressure of 6000-9000Pa and a temperature of 210-220 ℃ to obtain the second esterification solution.
8. The method as claimed in claim 1, wherein the esterification reaction is carried out on the heated reaction mixture at a residual vacuum pressure of 8000-9000Pa and a temperature of 200-210 ℃ to obtain the first esterification solution.
9. The method as claimed in claim 1, wherein the first esterification solution is subjected to esterification reaction at a vacuum residual pressure of 8000-9000Pa and a temperature of 210-215 ℃ to obtain the second esterification solution.
10. The method as claimed in claim 1, wherein the temperature of the reaction mixture is raised to 135 ℃ at first, to 175 ℃ at second and to 205 ℃ at last by using a U-shaped heat exchanger reactor.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804670A (en) * | 2012-11-08 | 2014-05-21 | 上海凯众材料科技股份有限公司 | Polyester diol synthesis process |
| CN104694256A (en) * | 2015-02-07 | 2015-06-10 | 铜仁学院 | Method for reducing acid value through catalyzing glycerol esterification with solid base |
| CN105038995A (en) * | 2015-08-21 | 2015-11-11 | 中国林业科学研究院林产化学工业研究所 | Non-catalytic esterification deacidification method for high-acid-value grease |
| CN107459997A (en) * | 2017-07-21 | 2017-12-12 | 中国林业科学研究院林产化学工业研究所 | A kind of high acid value waste oil glycerine is without catalytic esterification deacidification continuous production technology |
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2020
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804670A (en) * | 2012-11-08 | 2014-05-21 | 上海凯众材料科技股份有限公司 | Polyester diol synthesis process |
| CN104694256A (en) * | 2015-02-07 | 2015-06-10 | 铜仁学院 | Method for reducing acid value through catalyzing glycerol esterification with solid base |
| CN105038995A (en) * | 2015-08-21 | 2015-11-11 | 中国林业科学研究院林产化学工业研究所 | Non-catalytic esterification deacidification method for high-acid-value grease |
| CN107459997A (en) * | 2017-07-21 | 2017-12-12 | 中国林业科学研究院林产化学工业研究所 | A kind of high acid value waste oil glycerine is without catalytic esterification deacidification continuous production technology |
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