Device for separating and grading lignin from black liquor

Abstract

The utility model provides a device for separating and grading lignin from black liquor. A stirring device is arranged from the top to the bottom of the device in a penetrating manner; the device comprises a sample introduction part, a separation part and a discharge part which are sequentially arranged from top to bottom along the axial direction of the stirring device, wherein the number of the separation part is more than or equal to 1; the sample introduction part comprises a sample introduction tank and a sample introduction part mixer, and a heavy phase sample introduction port and a light phase outlet are formed in the side wall of the sample introduction part; the separation part comprises a separation tank and a separation part mixer; a clarified liquid outlet and a clarified liquid inlet are formed in the side wall of the separation tank; the discharging part comprises a discharging tank, and a heavy liquid outlet and a light liquid inlet are formed in the side wall of the discharging tank; the stirring device comprises a stirring shaft and at least two stirring parts, and the stirring parts are respectively in one-to-one correspondence with the sample introduction part mixer and the separation part mixer.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the technical field of separation device, especially to a device for separating and grading lignin from black liquor. BACKGROUND

[0002] Lignin is the second largest biomass resource next to cellulose, which is a polymer composed of p-hydroxyphenylpropane, guaiacylpropane and syringylpropane three basic monomers. It is widely present in various plants, and due to its unique aromatic structure and rich functional groups such as carbonyl, carboxyl and phenolic hydroxyl, lignin has broad application prospects.

[0003] The lignin extracted from black liquor in acid cooking is mainly separated by adjusting pH. This method has the disadvantages of large amount of wastewater, uneven particle size distribution due to easy polymerization of lignin, and easy inclusion of sugars during polymerization, resulting in high impurity content and low purity of lignin.

[0004] CN116837655A discloses a method for efficiently extracting bio-oil, lignin and recovering alkali from papermaking dilute black liquor, which comprises the following steps: S1 adjusting pH value; S2 centrifugal separation to obtain acid precipitation and acid precipitation waste liquid; S3: adding anhydrous organic solvent to the acid precipitation and mixing, centrifuging to obtain purified lignin and biomass fuel containing organic solvent; S4: adding anhydrous ethanol or anhydrous methanol to the acid precipitation waste liquid for extraction, and centrifuging to obtain liquid phase, organic matter and water mixture and inorganic salt precipitate; S5: recycling the corresponding alcohol solvent after recovering the corresponding alcohol solvent from the liquid phase obtained in S4, and then extracting the remaining material with an organic solvent and recovering the organic matter by reduced pressure distillation, and finally obtaining solid flocculate by calcium flocculation treatment of the remaining wastewater.

[0005] CN103074790A discloses a method for comprehensive utilization of cellulose, hemicellulose and lignin in biomass raw materials. The method is to cook the biomass raw materials with a mixture of formic acid and acetic acid under the catalytic action of hydrogen peroxide, so as to extract cellulose, lignin and hemicellulose respectively, and obtain cellulose, lignin and xylose.

[0006] The lignin extracted from black liquor in acid cooking has the disadvantages of complex structure, wide molecular weight distribution and deep color, which limits its high-value application. Therefore, preparing lignin with uniform molecular weight and light color by lignin grading is one of the main solutions to transform lignin into a high-value material. UTILITY MODEL CONTENT

[0007] In view of the deficiencies of the prior art, the device for separating and grading lignin from black liquor can simultaneously realize extraction of black liquor and separation of organic acid and extractant in the black liquor, and obtain lignin.

[0008] To achieve the above object, the device for separating and grading lignin from black liquor comprises the following technical solutions:

[0009] The device for separating and grading lignin from black liquor comprises a stirring device arranged from top to bottom.

[0010] The device comprises a sample inlet part, a separation part and a discharge part arranged in sequence from top to bottom along the axial direction of the stirring device, and the number of the separation part is greater than or equal to 1.

[0011] The sample inlet part comprises a sample inlet tank and a sample inlet part mixer, the sample inlet tank is close to the top of the device, the sample inlet part mixer is close to the bottom of the device, and a heavy phase sample inlet and a light phase outlet are arranged on the side wall of the sample inlet part.

[0012] The separation part comprises a separation tank and a separation part mixer, the separation tank is close to the top of the device, the separation part mixer is close to the bottom of the device, and a clarified liquid outlet and a clarified liquid inlet are arranged on the side wall of the separation tank.

[0013] The discharge part comprises a discharge tank, and a heavy liquid outlet and a light liquid inlet are arranged on the side wall of the discharge tank.

[0014] The stirring device comprises a stirring shaft and at least two stirring parts, and the stirring parts correspond to the sample inlet part mixer and the separation part mixer one by one.

[0015] In the device for separating and grading lignin from black liquor, the heavy phase sample inlet is used for black liquor feeding, the light liquid inlet is used for extractant feeding, the acid concentration of the black liquor is reduced under the action of the sample inlet part mixer and the stirring device, part of the lignin is precipitated and discharged from the light phase outlet, when the black liquor passes through the separation part, the acid concentration of the black liquor is further reduced under the action of the stirring device, the lignin is precipitated and deposited in the separation tank, and the lignin is separated after being precipitated to a certain degree. After the treatment of the above-mentioned structural units, most of the lignin has been precipitated, and the black liquor from which the lignin is separated is discharged from the heavy liquid outlet and stored.

[0016] The device for separating and grading lignin from black liquor can simultaneously realize extraction of black liquor and separation of extractant and organic acid in the device, reduce the content of organic acid in the black liquor, and realize separation and grading of lignin.

[0017] The filter plate is arranged in the sample inlet tank.

[0018] The filter plate can play a blocking role, and the separated lignin and the light phase are discharged through the light phase outlet.

[0019] The light phase outlet is connected with the conveying device and the filter through a pipeline in sequence.

[0020] The inner side wall of the sample inlet mixer and the inner side wall of the separation mixer are respectively provided with at least one static ring.

[0021] The inner side wall of the sample inlet mixer and the inner side wall of the separation mixer are respectively provided with at least one static ring.

[0022] The edge of the stirring disc is staggered with the static ring.

[0023] The stirring shaft penetrates the center of the stirring disc in the sample inlet mixer and the separation mixer.

[0024] The stirring device further comprises a motor.

[0025] The filter plate is arranged in the sample inlet tank.

[0026] The clarified liquid outlet is close to the bottom of the device, and the clarified liquid inlet is close to the top of the device.

[0027] The clarified liquid outlet is connected with the conveying device, the filter and the clarified liquid inlet in sequence through a pipeline.

[0028] The filter plate can play a blocking role, and the separated lignin and the light phase are discharged through the light phase outlet.

[0029] The numerical range of the present application includes not only the point values exemplified above, but also any point values between the above numerical ranges which are not exemplified.

[0030] Compared with the prior art, the device has the beneficial effects that:

[0031] The device can extract organic acids in the black liquor by using an extractant, so that the content of the organic acids in the black liquor is gradually reduced, thereby separating and grading lignin; the lignin obtained by using the device has uniform molecular weight and less impurities such as sugars, and the lignin has no self-polymerization phenomenon in the separation process. BRIEF DESCRIPTION OF DRAWINGS

[0032] Figure 1 A device for separating and grading lignin from black liquor provided by the utility model is shown in the schematic diagram, wherein 1 is a stirring device, 2 is a heavy phase sampling inlet, 3 is a sampling tank, 4 is a light phase outlet, 5 is a first filter plate, 6 is a first static ring, 7 is a first stirring area, 8 is a first stirring turntable, 9 is a first clarified liquid inlet, 10 is a second filter plate, 11 is a first clarified liquid outlet, 12 is a first separation tank, 13 is a second filter, 14 is a second static ring, 15 is a second stirring area, 16 is a second stirring turntable, 17 is a second clarified liquid inlet, 18 is a second clarified liquid outlet, 19 is a third filter plate, 20 is a second separation tank, 21 is a third static ring, 22 is a third stirring area, 23 is a third stirring turntable, 24 is a heavy liquid outlet, 25 is a second conveying device, 26 is a third filter, 27 is a light liquid inlet, 28 is a third connecting conveying device, 29 is a first filter, 30 is a first conveying device, and 31 is a discharge tank. DETAILED DESCRIPTION

[0033] It should be understood that, in the description of the utility model, the orientation or positional relationship indicated by the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the utility model and simplifying the description, and therefore cannot be understood as indicating or implying that the indicated device or element must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the utility model. In addition, the terms "first", "second" and the like are only for the purpose of description, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features limited by "first", "second" and the like can explicitly or implicitly include one or more features. In the description of the utility model, unless otherwise stated, the meaning of "multiple" is two or more.

[0034] It should be noted that in the description of the utility model, unless there is another explicit provision and limitation, the terms "arrangement", "connection", "connection" should be understood broadly, for example, it can be fixed connection, or detachable connection, or integral connection, it can be mechanical connection, or electrical connection, it can be directly connected, or indirectly connected through intermediate medium, it can be the communication inside two elements. For ordinary skilled in the art, the specific meaning of the above terms in the utility model can be understood through specific circumstances.

[0035] The technical scheme of the utility model will be further illustrated below by specific embodiments in conjunction with the drawings.

[0036] In one specific embodiment, the utility model provides a device for separating and grading lignin from black liquor, the structural schematic diagram of the device is as shown in Figure 1 The top to the bottom of the device is provided with a stirring device 1;

[0037] The device comprises a sample inlet portion, a first separation portion, a second separation portion and a discharge portion arranged in sequence from top to bottom along the axial direction of the stirring device 1, and the number of the separation portions is 2.

[0038] The sample inlet portion comprises a sample inlet tank 3 and a sample inlet portion mixer, the sample inlet tank 3 is close to the top of the device, and the sample inlet portion mixer is close to the bottom of the device, and a heavy phase inlet port 2 and a light phase outlet port 4 are arranged on the side wall of the sample inlet portion;

[0039] The first separation portion comprises a first separation tank 12 and a first separation portion mixer, the first separation tank 12 is close to the top of the device, and the separation portion mixer is close to the bottom of the device, and a first clarified liquid outlet port 11 and a first clarified liquid inlet port 9 are arranged on the side wall of the first separation tank;

[0040] The second separation portion comprises a second separation tank 20 and a second separation portion mixer, the second separation tank 20 is close to the top of the device, and the separation portion mixer is close to the bottom of the device, and a second clarified liquid outlet port 18 and a second clarified liquid inlet port 17 are arranged on the side wall of the second separation tank;

[0041] The discharge portion comprises a discharge tank 31, and a heavy liquid outlet port 24 and a light liquid inlet port 27 are arranged on the side wall of the discharge tank;

[0042] The stirring device comprises a stirring shaft and three stirring portions, and the stirring portions correspond to the sample inlet portion mixer, the first separation portion mixer and the second separation portion mixer one by one.

[0043] The utility model discloses a device is separated and graded lignin from black liquor, and the heavy phase sampling port is used for black liquor feed, and the light liquid import is used for extractant feed, and black liquor passes through the sampling part mixer, under the action of stirring device, the acid concentration of black liquor reduces, and part lignin precipitates, and is discharged by the light phase export.

[0044] The device for separating and grading lignin from black liquor can simultaneously realize extraction of black liquor and separation of extractant and organic acid in the device, reduces the content of organic acid in the black liquor, and realizes separation and grading of lignin.

[0045] Further, the inside of the sampling tank 3 is provided with a first filter plate 5.

[0046] In the sampling tank of the device for separating and grading lignin from black liquor, the filter plate can play a blocking role, and the precipitated lignin and the light phase are discharged together through the light phase export, and lignin is obtained through separation.

[0047] Further, the light phase export 4 is connected with a first conveying device 30 and a first filter 29 through a pipeline in sequence.

[0048] Further, the inside side wall of the sampling part mixer, the first separation part mixer and the second separation part mixer is respectively provided with a first static ring 6, a second static ring 14 and a third static ring 21.

[0049] Further, the inside of the sampling part mixer, the first separation part mixer and the second separation part mixer is respectively provided with a first stirring zone 7, a second stirring zone 15 and a third stirring zone 22.

[0050] Further, the inside of the sampling part mixer, the first separation part mixer and the second separation part mixer is respectively provided with a first stirring turntable 8, a second stirring turntable 16 and a third stirring turntable 23.

[0051] Further, the edge of the first stirring turntable 8 is staggered with the first static ring 6, the edge of the second stirring turntable 16 is staggered with the second static ring 14, and the edge of the third stirring turntable 23 is staggered with the third static ring 21.

[0052] Further, the stirring shaft penetrates the center of the first stirring turntable 8, the second stirring turntable 16 and the third stirring turntable 23 in the inside of the sampling part mixer, the first separation part mixer and the second separation part mixer.

[0053] Further, the stirring device also includes a motor.

[0054] Further, the inside of the first separation tank 12 and the second separation tank 20 is respectively provided with a second filter plate 10 and a third filter plate 19.

[0055] Further, the first clarified liquid outlet 11 is close to the bottom of the device, and the first clarified liquid inlet 9 is close to the top of the device.

[0056] Further, the second clarified liquid outlet 18 is close to the bottom of the device, and the second clarified liquid inlet 17 is close to the top of the device.

[0057] Further, the first clarified liquid outlet 11 is sequentially connected with the second conveying device 25, the second filter 13 and the first clarified liquid outlet inlet 9 through pipelines.

[0058] Further, the second clarified liquid outlet 18 is sequentially connected with the third conveying device 28, the third filter 26 and the second clarified liquid outlet inlet 17 through pipelines.

[0059] The filter plate in the separation tank of the device for separating and grading lignin from black liquor can play a blocking role, lignin is precipitated on the filter plate, and the precipitated lignin is pumped out to the filter for separation to obtain lignin after being deposited to a certain degree, and the filtrate is returned to the device through the clarified liquid inlet.

[0060] Embodiment 1

[0061] The embodiment provides a device for separating and grading lignin from black liquor, and a structural schematic diagram of the device is as shown in Figure 1 The top to the bottom of the device is provided with a stirring device 1;

[0062] The device includes a sampling part, a first separation part, a second separation part and a discharge part which are sequentially arranged from top to bottom along the axial direction of the stirring device 1.

[0063] The sampling part includes a sampling tank 3 and a sampling part mixer, the inside of the sampling tank 3 is provided with a first filter plate 5, the sampling tank 3 is close to the top of the device, the sampling part mixer is close to the bottom of the device, a heavy phase sampling inlet 2 and a light phase outlet 4 are arranged on the side wall of the sampling part, the light phase outlet 4 is sequentially connected with a first conveying device 30 and a first filter 29 through pipelines. A first static ring 6 is arranged on the inner side wall of the sampling part mixer, and a first stirring zone 7 and a first stirring turntable 8 are arranged in the sampling part mixer, wherein the edge of the first stirring turntable 8 is staggered with the first static ring 6.

[0064] The first separation part comprises a first separation tank 12 and a first separation part mixer, the first separation tank 12 is close to the top of the device, the separation part mixer is close to the bottom of the device, the inside of the first separation tank 12 is provided with a second filter plate 10, the sidewall of the first separation tank 12 is provided with a first clarified liquid outlet 11 and a first clarified liquid inlet 9, the first clarified liquid outlet 11 is close to the bottom of the device, the first clarified liquid inlet 9 is close to the top of the device, the first clarified liquid outlet 11 is sequentially connected with a second conveying device 25, a second filter 13 and a first clarified liquid outlet and inlet 9 through a pipeline, the inside sidewall of the first separation part mixer is provided with a second static ring 14, the inside of the first separation part mixer is provided with a second stirring area 15 and a second stirring turntable 16, wherein the edge of the second stirring turntable 16 is staggered with the second static ring 14.

[0065] The second separation part comprises a second separation tank 20 and a second separation part mixer, the second separation tank 20 is close to the top of the device, the separation part mixer is close to the bottom of the device, the inside of the second separation tank 20 is provided with a third filter plate 19, the sidewall of the second separation tank 20 is provided with a second clarified liquid outlet 18 and a second clarified liquid inlet 17, the second clarified liquid outlet 18 is close to the bottom of the device, the second clarified liquid inlet 17 is close to the top of the device, the second clarified liquid outlet 18 is sequentially connected with a third conveying device 28, a third filter 26 and a second clarified liquid outlet and inlet 17 through a pipeline, the inside sidewall of the second separation part mixer is provided with a third static ring 21, the inside of the second separation part mixer is provided with a third stirring area 22 and a third stirring turntable 23, wherein the edge of the third stirring turntable 23 is staggered with the third static ring 21.

[0066] The stirring device comprises a stirring shaft and a motor, the stirring shaft penetrates the center of the first stirring turntable 8, the second stirring turntable 16 and the third stirring turntable 23 inside the sample inlet part mixer, the first separation part mixer and the second separation part mixer.

[0067] Application Example 1

[0068] In this application example, the device described in Example 1 is used to separate and fractionate lignin from black liquor, and n-butyl acetate is used as the extractant.

[0069] Comparative Application Example 1

[0070] In this comparative example, a conventional single tank is used, water is added to the black liquor to reduce the acid concentration to pH 2-3 to precipitate lignin.

[0071] The lignin obtained by the application example 1 and the comparative application example 1 is tested, wherein the larger the brightness index L is, the lighter the color is, and the higher the purity is, and the test results are shown in Table 1:

[0072] Table 1

[0073]

[0074] It can be seen from the above Table 1 that the device for separating and grading lignin from black liquor can realize the separation and grading of lignin, and the lignin obtained by each filter is uniform in molecular weight, light in color and high in purity.

[0075] The applicant declares that the above is only a specific embodiment of the present application, but the protection scope of the present application is not limited thereto, and those skilled in the art should understand that any changes or replacements easily thought of by those skilled in the art within the technical scope disclosed by the present application fall within the protection scope and disclosure scope of the present application.

Claims

1. A device for separating and fractionating lignin from black liquor, characterized in that: A stirring device is provided from the top to the bottom of the device; The device comprises a sample introduction part, a separation part and a material discharge part arranged in sequence from the top to the bottom along the axial direction of the stirring device, and the number of the separation parts is ≥1; The sampling part includes a sampling tank and a sampling mixer, wherein the sampling tank is close to the top of the device, the sampling mixer is close to the bottom of the device, and a heavy phase inlet and a light phase outlet are provided on the side wall of the sampling part; The separation part includes a separation tank and a separation part mixer, the separation tank is close to the top of the device, the separation part mixer is close to the bottom of the device, and a clarified liquid outlet and a clarified liquid inlet are provided on the side wall of the separation tank; The discharge part includes a discharge tank, and a heavy liquid outlet and a light liquid inlet are provided on the side wall of the discharge tank; The stirring device comprises a stirring shaft and at least two stirring parts, and the stirring parts correspond to the sample injection part mixer and the separation part mixer one by one.

2. The device for separating and fractionating lignin from black liquor according to claim 1, characterized in that A filter plate is arranged inside the sample injection tank.

3. The device for separating and fractionating lignin from black liquor according to claim 1, characterized in that The light phase outlet is connected to a conveying device and a filter through pipelines in sequence.

4. The device for separating and fractionating lignin from black liquor according to claim 1, characterized in that At least one static ring is respectively provided on the inner side wall of the injection part mixer and the separation part mixer; A stirring zone and at least one stirring turntable are respectively arranged inside the sample injection part mixer and the separation part mixer.

5. The device for separating and fractionating lignin from black liquor according to claim 4, characterized in that The edge of the stirring turntable and the static ring are arranged alternately.

6. The device for separating and fractionating lignin from black liquor according to claim 5, characterized in that The stirring shaft passes through the center of the stirring turntable inside the sample introduction part mixer and the separation part mixer.

7. The device for separating and fractionating lignin from black liquor according to claim 1, characterized in that The stirring device also includes a motor.

8. The device for separating and fractionating lignin from black liquor according to claim 1, characterized in that A filter plate is arranged inside the separation tank.

9. The device for separating and fractionating lignin from black liquor according to claim 1, characterized in that The clarified liquid inlet is located near the top of the device.

10. The device for separating and fractionating lignin from black liquor according to claim 9, characterized in that The clarified liquid outlet is sequentially connected to the conveying device, the filter and the clarified liquid inlet and outlet through pipelines.

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