阅读说明：本技术 一种利用甘油连续酯化餐厨废弃油酯的装置及方法 (Device and method for continuously esterifying kitchen waste oil ester by using glycerol ) 是由 赵敏仲 王子腾 刘少杰 褚晓萌 赵松 赵龙 于 2021-07-26 设计创作，主要内容包括：本发明公开了一种利用粗甘油连续酯化餐厨废弃油酯的装置及方法,装置包括粗甘油储罐、餐厨废弃油酯储罐、多级酯化釜、多级静态混合器和酯化后的餐厨废弃油酯储罐；粗甘油储罐和餐厨废弃油酯储罐分别与多级静态混合器连接；多级静态混合器依次与多级酯化釜、酯化后的餐厨废弃油酯储罐连接。本发明中的装置结构简单,经过多级酯化釜酯化后的餐厨废弃油酯中的硫含量得到了显著的降低,从而降低了生物柴油生产过程中的脱硫成本。(The invention discloses a device and a method for continuously esterifying kitchen waste grease by using crude glycerol, wherein the device comprises a crude glycerol storage tank, a kitchen waste grease storage tank, a multistage esterification kettle, a multistage static mixer and an esterified kitchen waste grease storage tank; the crude glycerol storage tank and the kitchen waste grease storage tank are respectively connected with a multistage static mixer; the multistage static mixer is connected with the multistage esterification kettle and the esterified kitchen waste grease storage tank in sequence. The device provided by the invention is simple in structure, and the sulfur content in the kitchen waste oil ester esterified by the multi-stage esterification kettle is remarkably reduced, so that the desulfurization cost in the biodiesel production process is reduced.)

1. A device for continuously esterifying kitchen waste grease by using crude glycerol is characterized by comprising a crude glycerol storage tank, a kitchen waste grease storage tank, a multistage esterification kettle, a multistage static mixer and an esterified kitchen waste grease storage tank;

the crude glycerol storage tank and the kitchen waste grease storage tank are respectively connected with a multistage static mixer;

the multistage static mixer is sequentially connected with the multistage esterification kettle and the esterified kitchen waste grease storage tank.

2. The device for continuously esterifying kitchen waste oil ester by using crude glycerol according to claim 1, wherein the multistage esterification kettle comprises a first-stage esterification kettle, a second-stage esterification kettle, a third-stage esterification kettle and a fourth-stage esterification kettle;

the kitchen waste grease storage tank is sequentially connected with the first-stage esterification kettle, the second-stage esterification kettle, the third-stage esterification kettle and the fourth-stage esterification kettle.

3. The device for continuously esterifying kitchen waste oil ester by using crude glycerol according to claim 2, wherein the multistage static mixer comprises a first-stage static mixer, a second-stage static mixer, a third-stage static mixer and a fourth-stage static mixer;

one end of the primary static mixer is respectively connected with the crude glycerine storage tank and the kitchen waste grease storage tank, and the other end of the primary static mixer is connected with the top end of the primary esterification kettle;

the second grade static mixer in proper order with the second grade static mixer the second grade esterification cauldron the tertiary static mixer the tertiary esterification cauldron the level four static mixer the level four esterification cauldron is connected the kitchen waste oil ester storage tank after esterifying connects.

4. The device for continuously esterifying kitchen waste oil ester by using crude glycerol according to claim 3, further comprising: a plurality of circulation pumps; the one-level esterification kettle with between the second grade static mixer, the second grade esterification kettle with between the tertiary static mixer, tertiary esterification kettle with between the level four static mixer, level four esterification kettle with all be equipped with the circulating pump between the kitchen waste oil ester storage tank after esterifying.

5. A method for continuous esterification of waste kitchen oil esters with raw glycerol using a device according to any of claims 1 to 4, characterized in that it comprises the following steps:

heating the crude glycerine in the crude glycerine storage tank and the kitchen waste grease in the kitchen waste grease storage tank, then entering a multistage static mixer through a pipeline to be uniformly mixed, entering a multistage esterification kettle to be stirred and heated for esterification, obtaining the kitchen waste grease after esterification and storing the kitchen waste grease in the kitchen waste grease storage tank after esterification.

6. The method for continuously esterifying kitchen waste oil ester by using crude glycerol according to claim 5, wherein the mass ratio of the crude glycerol to the kitchen waste oil ester is (2-4): 100, the water impurity of the kitchen waste oil ester is less than 1%;

the heating temperature is 150-180 ℃.

7. The method for continuously esterifying kitchen waste oil ester by using crude glycerol according to claim 5, wherein the stirring and heating speed is 30-60r/min, and the time is 80-100 min.

8. The method for continuously esterifying kitchen waste oil ester by using crude glycerol according to claim 5, wherein the acid value of the esterified kitchen waste oil ester is less than 0.3mgKOH/g, and the sulfur content is 30-50 PPM.

Technical Field

The invention relates to the technical field of kitchen waste oil transesterification, in particular to a device and a method for continuously esterifying kitchen waste oil by using glycerol.

Background

The kitchen waste grease refers to various inferior oils in life, such as recovered edible oil, repeatedly used frying oil and the like, the largest source of the kitchen waste grease is an oil separation tank of a sewer of a large-scale urban restaurant, and the kitchen waste grease can cause cancers after being eaten for a long time and is extremely harmful to human bodies; the kitchen waste grease is used as a raw material, and is processed into the biodiesel with high efficiency and low cost through chemical engineering, so that the kitchen waste grease can become a favorable industrial resource, but in the process of preparing the biodiesel by utilizing the waste grease principle of the kitchen waste grease, acidified oil and the like, how to remove free fatty acid in the grease raw material is a difficult point in the preparation process and a key point of process technology.

At present, when the kitchen waste oil ester is used for producing biodiesel in the market, acid catalysis esterification is needed, acid residues generated by acid catalysis can generate a carbonization effect on grease, so that the color and luster of the biodiesel product are poor, and the product quality is influenced; has corrosive effect on equipment, cannot use a conventional stainless steel reaction vessel, also causes environmental pollution and becomes a great problem for biodiesel enterprises.

Therefore, the problem to be solved by those skilled in the art is how to provide a device and a method for continuously esterifying kitchen waste oil ester by using glycerol without a catalyst and acid waste residues.

Disclosure of Invention

In view of the above, the invention provides a device and a method for continuously esterifying kitchen waste oil ester by using glycerol.

In order to achieve the purpose, the invention adopts the following technical scheme: a device for continuously esterifying kitchen waste grease by using crude glycerol is characterized by comprising a crude glycerol storage tank, a kitchen waste grease storage tank, a multistage esterification kettle, a multistage static mixer and an esterified kitchen waste grease storage tank;

the crude glycerol storage tank and the kitchen waste grease storage tank are respectively connected with a multistage static mixer;

the multistage static mixer is sequentially connected with the multistage esterification kettle and the esterified kitchen waste grease storage tank.

The device provided by the invention is simple in structure, and the sulfur content in the kitchen waste oil ester esterified by the multi-stage esterification kettle is remarkably reduced, so that the desulfurization cost in the biodiesel production process is reduced.

Preferably, the multistage esterification kettle comprises a first-stage esterification kettle, a second-stage esterification kettle, a third-stage esterification kettle and a fourth-stage esterification kettle;

the kitchen waste grease storage tank is sequentially connected with the first-stage esterification kettle, the second-stage esterification kettle, the third-stage esterification kettle and the fourth-stage esterification kettle.

Preferably, the multistage static mixer comprises a first-stage static mixer, a second-stage static mixer, a third-stage static mixer and a fourth-stage static mixer;

one end of the primary static mixer is respectively connected with the crude glycerine storage tank and the kitchen waste grease storage tank, and the other end of the primary static mixer is connected with the top end of the primary esterification kettle;

the second grade static mixer in proper order with the second grade static mixer the second grade esterification cauldron the tertiary static mixer the tertiary esterification cauldron the level four static mixer the level four esterification cauldron is connected the kitchen waste oil ester storage tank after esterifying connects.

Preferably, the method further comprises the following steps: a plurality of circulation pumps; the one-level esterification kettle with between the second grade static mixer, the second grade esterification kettle with between the tertiary static mixer, tertiary esterification kettle with between the level four static mixer, level four esterification kettle with all be equipped with the circulating pump between the kitchen waste oil ester storage tank after esterifying.

The invention also provides a method for continuously esterifying the kitchen waste oil ester by using the crude glycerol, which comprises the following steps:

heating the crude glycerine in the crude glycerine storage tank and the kitchen waste grease in the kitchen waste grease storage tank, then entering a multistage static mixer through a pipeline to be uniformly mixed, entering a multistage esterification kettle to be stirred and heated for esterification, obtaining the kitchen waste grease after esterification and storing the kitchen waste grease in the kitchen waste grease storage tank after esterification.

Preferably, the mass ratio of the crude glycerol to the kitchen waste oil ester is (2-4): 100, the water impurity of the kitchen waste oil ester is less than 1%;

the heating temperature is 150-180 ℃.

Preferably, the stirring and heating speed is 30-60r/min, and the time is 80-100 min.

Preferably, the acid value of the esterified kitchen waste oil ester is less than 0.3mgKOH/g, and the sulfur content is 30-50 PPM.

According to the technical scheme, compared with the prior art, the device and the method for continuously esterifying the kitchen waste oil ester by using the glycerol have the following beneficial effects that:

1. avoids acid catalysis, and does not produce acid sludge to cause secondary pollution.

2. The sulfur content in the kitchen waste oil ester subjected to continuous glycerin esterification can be reduced, the sulfur content of the kitchen waste oil ester is 400PPM which is 300-fold of the sulfur content of the kitchen waste oil ester, and the sulfur content of the kitchen waste oil ester subjected to glycerin esterification is 30-50PPM, so that the method is very beneficial to a biodiesel process, and the desulfurization cost in the biodiesel production process is reduced.

3. Compared with a continuous medium-pressure non-catalytic esterification process, the process has low energy consumption and does not need to vaporize a large amount of high-temperature methanol under pressure.

4. The glycerol adopted in the invention is a byproduct from the production process of biodiesel, the glycerol is recycled, part of the glycerol is generated by acid catalysis and cannot be recovered in acid sludge, and the glycerol of the kitchen waste oil ester after the esterification of the adopted crude glycerol can be refined into the glycerol with the content of 99%, so that the additional value of the product is increased.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.

FIG. 1 is a schematic diagram of the structure provided by the present invention;

wherein, 1-a crude glycerol storage tank, 2-a kitchen waste grease storage tank, 5-an esterified kitchen waste grease storage tank, 6-a circulating pump I, 7-a circulating pump II, 8-a circulating pump III and 9-a circulating pump IV;

31-a first-stage esterification kettle, 32-a second-stage esterification kettle, 33-a third-stage esterification kettle and 34-a fourth-stage esterification kettle;

41-first-stage static mixer, 42-second-stage static mixer, 43-third-stage static mixer and 44-fourth-stage static mixer.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The device for continuously esterifying the kitchen waste grease by using the crude glycerol comprises a crude glycerol storage tank 1, a kitchen waste grease storage tank 2, a multistage esterification kettle, a multistage static mixer and an esterified kitchen waste grease storage tank 5;

the crude glycerol storage tank 1 and the kitchen waste oil ester storage tank 2 are respectively connected with a multistage static mixer;

the multistage static mixer is connected with the multistage esterification kettle and the esterified kitchen waste grease storage tank 5 in sequence.

In one embodiment, the multistage esterification kettle comprises a first-stage esterification kettle 31, a second-stage esterification kettle 32, a third-stage esterification kettle 33 and a fourth-stage esterification kettle 34;

the kitchen waste oil ester storage tank 2 is sequentially connected with a primary esterification kettle 31, a secondary esterification kettle 32, a tertiary esterification kettle 33 and a quaternary esterification kettle 34;

the upper end of each esterification kettle is provided with a condenser pipe which is connected with a vacuum cooling device.

In one embodiment, the multistage static mixer includes a first-stage static mixer 41, a second-stage static mixer 42, a third-stage static mixer 43, a fourth-stage static mixer 44;

one end of the primary static mixer 41 is respectively connected with the crude glycerol storage tank 1 and the kitchen waste grease storage tank 2, and the other end is connected with the top end of the primary esterification kettle 31;

the second-stage static mixer 42 is connected with the second-stage static mixer 42, the second-stage esterification kettle 32, the third-stage static mixer 43, the third-stage esterification kettle 33, the fourth-stage static mixer 44 and the fourth-stage esterification kettle 34 in sequence, and the esterified kitchen waste oil ester storage tank 5 is connected with the second-stage static mixer 42.

In one embodiment, further comprising: a plurality of circulation pumps; circulating pumps are arranged between the first-stage esterification kettle 31 and the second-stage static mixer 42, between the second-stage esterification kettle 32 and the third-stage static mixer 43, between the third-stage esterification kettle 33 and the fourth-stage static mixer 44, and between the fourth-stage esterification kettle 34 and the esterified kitchen waste oil ester storage tank 5.

The method for continuously esterifying the kitchen waste oil ester by using crude glycerol comprises the following steps:

heating the crude glycerol in the crude glycerol storage tank 1 and the kitchen waste grease in the kitchen waste grease storage tank 2 to 180 ℃ according to the mass ratio of the crude glycerol to the kitchen waste grease storage tank 2 being 4:100, enabling the crude glycerol and the kitchen waste grease to enter a primary static mixer 41 through a pipeline to be uniformly mixed, enabling the mixture to enter a primary esterification kettle 31 through a pipeline, stirring the mixture for 90min at the speed of 60r/min, and controlling the pressure to be normal pressure through a vacuum cooling device to obtain a mixed solution I;

according to the mass ratio of 4:100 of crude glycerol to the mixed solution I, pumping the mixed solution I and the crude glycerol with the temperature of 180 ℃ into a secondary static mixer 42 through a circulating pump I6, uniformly feeding the mixed solution I and the crude glycerol into a secondary esterification kettle 32, heating the mixed solution I and the crude glycerol to 200 ℃, stirring the mixed solution I and the crude glycerol for 90min at the speed of 60r/min, and simultaneously controlling the pressure of a vacuum cooling device to be normal pressure to obtain a mixed solution II;

pumping the crude glycerol and the mixed solution II into a three-stage static mixer 43 through a circulating pump II 7 according to the mass ratio of the crude glycerol to the mixed solution II being 4:100, keeping the temperature at 180 ℃, uniformly mixing, then feeding into a three-stage esterification kettle 33, heating to 230 ℃, stirring for 90min at the speed of 60r/min, and simultaneously controlling the pressure to be-0.5 MPa through a vacuum cooling device to obtain a mixed solution III;

according to the mass ratio of 4:100 of the crude glycerol to the mixed liquid III, pumping the crude glycerol and the mixed liquid III into a four-stage static mixer 44 through a circulating pump III 8, keeping the temperature at 180 ℃, uniformly mixing, then feeding into a four-stage esterification kettle 34, heating to 260 ℃, stirring for 90min at the speed of 60r/min, simultaneously controlling the pressure to be-0.9 MPa through a vacuum cooling device, and finally pumping into an esterified kitchen waste oil ester storage tank 5 through a circulating pump IV 9.

Example 2

The device for continuously esterifying the kitchen waste oil ester by using the crude glycerol is the same as the embodiment 1;

the method for continuously esterifying the kitchen waste oil ester by using crude glycerol comprises the following steps:

heating the crude glycerol in the crude glycerol storage tank 1 and the kitchen waste grease in the kitchen waste grease storage tank 2 to 150 ℃ according to the mass ratio of the crude glycerol to the kitchen waste grease 2 being 2:100, uniformly mixing the crude glycerol in a primary static mixer 41 through a pipeline, then feeding the mixture into a primary esterification kettle 31 through a pipeline, stirring the mixture for 90min at the speed of 30r/min, and controlling the pressure to be normal pressure through a vacuum cooling device to obtain a mixed solution I;

according to the mass ratio of 2:100 of the crude glycerol to the mixed solution I, pumping the mixed solution I and the crude glycerol with the temperature of 150 ℃ into a secondary static mixer 42 through a circulating pump I6, uniformly heating the mixed solution I and the crude glycerol to 180 ℃ in a secondary esterification kettle 32, stirring the mixed solution I and the crude glycerol for 90min at the speed of 30r/min, and simultaneously controlling the pressure to be normal pressure through a vacuum cooling device to obtain a mixed solution II;

pumping the crude glycerol and the mixed solution II into a three-stage static mixer 43 through a circulating pump II 7 according to the mass ratio of the crude glycerol to the mixed solution II of 2:100, keeping the temperature at 150 ℃, uniformly mixing, then heating to 200 ℃ in a three-stage esterification kettle 33, stirring for 90min at the speed of 30r/min, and simultaneously controlling the pressure to be-0.5 MPa through a vacuum cooling device to obtain a mixed solution III;

according to the mass ratio of the crude glycerol to the mixed liquid III of 2:100, pumping the crude glycerol and the mixed liquid III into a four-stage static mixer 44 through a circulating pump III 8, keeping the temperature at 150 ℃, uniformly mixing, then feeding into a four-stage esterification kettle 34, heating to 230 ℃, stirring for 90min at the speed of 30r/min, simultaneously controlling the pressure to be-0.9 MPa through a vacuum cooling device, and finally pumping into an esterified kitchen waste oil ester storage tank 5 through a circulating pump IV 9.

Example 3

The device for continuously esterifying the kitchen waste oil ester by using the crude glycerol is the same as the embodiment 1;

the method for continuously esterifying the kitchen waste oil ester by using crude glycerol comprises the following steps:

heating the crude glycerol in the crude glycerol storage tank 1 and the kitchen waste oil ester in the kitchen waste oil ester storage tank 2 to 165 ℃ according to the mass ratio of the crude glycerol to the kitchen waste oil ester storage tank 2 being 3:100, allowing the crude glycerol and the kitchen waste oil ester to enter a primary static mixer 41 through a pipeline, uniformly mixing the crude glycerol and the kitchen waste oil ester, allowing the mixture to enter a primary esterification kettle 31 through a pipeline, stirring the mixture for 90min at the speed of 45r/min, and controlling the pressure to be normal pressure through a vacuum cooling device to obtain a mixed solution I;

according to the mass ratio of 3:100 of crude glycerol to the mixed solution I, pumping the mixed solution I and the crude glycerol with the temperature of 165 ℃ into a secondary static mixer 42 through a circulating pump I6, uniformly feeding the mixed solution I and the crude glycerol into a secondary esterification kettle 32, heating to 190 ℃, stirring for 90min at the speed of 45r/min, and simultaneously controlling the pressure to be normal pressure through a vacuum cooling device to obtain a mixed solution II;

pumping the crude glycerol and the mixed solution II into a three-stage static mixer 43 through a circulating pump II 7 according to the mass ratio of the crude glycerol to the mixed solution II of 3:100, keeping the temperature at 165 ℃, uniformly mixing, then heating to 215 ℃ in a three-stage esterification kettle 33, stirring for 90min at the speed of 45r/min, and simultaneously controlling the pressure to be-0.5 MPa through a vacuum cooling device to obtain a mixed solution III;

according to the mass ratio of 3:100 of the crude glycerol to the mixed liquid III, pumping the crude glycerol and the mixed liquid III into a four-stage static mixer 44 through a circulating pump III 8, keeping the temperature at 165 ℃, uniformly mixing, then feeding into a four-stage esterification kettle 34, heating to 245 ℃, stirring for 90min at the speed of 45r/min, simultaneously controlling the pressure to be-0.9 MPa through a vacuum cooling device, and finally pumping into an esterified kitchen waste oil ester storage tank 5 through a circulating pump IV 9.

Performance testing

Example 1-3 index comparison of kitchen waste oil esters before esterification and kitchen waste oil esters after esterification, table 1 below:

table 1 examples 1-3 performance test results of kitchen waste oil esters

From the above table, it can be seen that the sulfur content in the kitchen waste oil ester after the continuous esterification of glycerol is reduced.

The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.