Emulsion preparation method of high-dispersion modified lignin

Abstract

The invention provides a preparation method of a high-dispersion modified lignin emulsion, which mainly comprises the following steps: pouring lignin into a stainless steel cylinder, adding deionized water into the stainless steel cylinder, soaking the lignin in the deionized water, stirring, washing with water, carrying out suction filtration to remove the deionized water, and repeatedly carrying out suction filtration for 3-5 times to obtain the high-dispersion modified lignin emulsion. Keeping the washed lignin in the stainless steel cylinder; the stainless steel cylinder is a full-automatic batch treatment type multifunctional cylinder, and a mixing device integrating multiple functions of washing, suction filtration, mixing, drying, self-heating, self-cleaning and the like can be achieved through the blending cylinder; the structure size is small, one machine has multiple purposes, the function is powerful, lignin and various raw materials for modification are automatically put into the modulation cylinder in sequence according to the preparation steps, all the processes of lignin preparation are automatically completed, the modulation cylinder is small in occupied area, the interior of a mixing cavity can be automatically cleaned after a batch of lignin is prepared through batch treatment, and the operation is convenient. And the next batch of products are prevented from being polluted.

Description

Technical Field

[0001] The present invention relates to the technical field of lignin production and preparation, and specifically to a method for preparing an emulsion of highly dispersed modified lignin. Background Art

[0002] Lignin is a non-crystalline, highly branched three-dimensional network phenolic biopolymer containing aromatic rings, and lignin widely exists in higher plant cells. In nature, lignin is the second most abundant renewable natural polymer in the world, second only to cellulose. It is estimated that about 5×10^8 - 36×10^8 tons can be produced globally each year. In plants, lignin, together with cellulose, hemicellulose, etc., constitutes a supramolecular system. Lignin binds cellulose to enhance the mechanical strength of plants. The structure of lignin is complex. So far, although the complete structure of natural lignin has not been known, years of research have shown that lignin contains many active groups, such as aromatic groups, alcohol hydroxyl groups, carboxyl groups, methoxy groups, conjugated double bonds, etc., and has certain chemical activity;

[0003] Lignin can undergo grafting, cross-linking and other reactions with materials such as rubber and plastics. Moreover, the hydroxyl active groups in lignin can form aromatic hydrogen bonds with the π electron clouds of conjugated double bonds in rubber; the unshared electron pairs on the oxygen atoms in groups such as methoxy groups, hydroxyl groups and carbonyl groups can form lignin-metal chelates with metal ions in a coordination bond manner, and the reaction activity of lignin molecules is used to construct a cross-linked network structure, so that lignin plays a role in reinforcing and plasticizing.

[0004] Currently, there are also relevant patents disclosing methods for preparing modified lignin, but the preparation process involves multiple processes, and during the preparation process, lignin or lignin dispersion needs to be continuously transferred. Such operations make the lignin preparation require a large plant area, the device for preparing lignin has a complex structure, and the preparation efficiency is low, which is not suitable for small laboratories or small factories, etc. Summary of the Invention

[0005] Aiming at the problems in the prior art, the purpose of the present invention is to provide a method for preparing an emulsion of highly dispersed modified lignin, and solve the technical problems described in the above background art, that is, currently, there are also relevant patents disclosing methods for preparing modified lignin, but the preparation process involves multiple processes, and during the preparation process, lignin or lignin dispersion needs to be continuously transferred. Such operations make the lignin preparation require a large plant area, the device for preparing lignin has a complex structure, and the preparation efficiency is low, which is not suitable for small laboratories or small factories.

[0006] The technical problems to be solved by the present invention are realized by adopting the following technical solutions: A method for preparing an emulsion of highly dispersed modified lignin, and this method for preparing an emulsion of highly dispersed modified lignin mainly includes the following steps:

[0007] S1, Washing lignin: Pour lignin into a stainless-steel cylinder, then add deionized water into the stainless-steel cylinder, soak the lignin with deionized water and stir to wash, then filter to remove the deionized water. After repeating the filtration 3 - 5 times, keep the washed lignin in the stainless-steel cylinder;

[0008] S2, Preparing the dispersion: Add aqueous solution to the lignin retained in the stainless-steel cylinder to obtain a lignin dispersion with a certain mass concentration, and control the pH value of the lignin dispersion to be 7 - 8;

[0009] S3, Heating and emulsifying: Heat the bottom of the stainless-steel cylinder to a certain temperature, then continuously stir the lignin dispersion in the stainless-steel cylinder. During the stirring process, evenly drip emulsifier and emulsion stabilizer into the stainless-steel cylinder, and keep the stirring speed during the dripping process;

[0010] S4, Heating and injecting liquid wax: Continue to heat the bottom of the stainless-steel cylinder to increase the temperature inside the stainless-steel cylinder. During the temperature increase process, synchronously accelerate the stirring speed of the lignin dispersion inside the stainless-steel cylinder and maintain for a certain time to obtain an emulsion of highly dispersed modified lignin;

[0011] S5, Drying to obtain powder: Dry the emulsion inside the stainless-steel cylinder by thermal drying. During the drying process, continuously stir the inside of the stainless-steel cylinder to obtain highly dispersed modified lignin particle powder;

[0012] S6, Discharging and cooling: Discharge the obtained highly dispersed modified lignin particle powder from inside the stainless-steel cylinder, and then quickly cool it to room temperature (below 25°C), then the production and preparation of highly dispersed modified lignin can be completed.

[0013] As a preferred technical solution of the present invention, the above-described steps S1 - S5 are mainly completed in cooperation with an emulsion device for highly dispersed modified lignin. The emulsion device for highly dispersed modified lignin includes a modulation cylinder, the modulation cylinder is set as a cylindrical structure, there is a mixing chamber inside the modulation cylinder, a cylinder cover plate is installed at the top of the modulation cylinder, a rotating stirring rod is arranged in the middle at the bottom of the cylinder cover plate, a lifting paddle is arranged at the bottom of the stirring rod, a feed pipe is connected to the outer wall of the modulation cylinder, the feed pipe extends into the upper part of the mixing chamber, a discharge port is connected to the outer wall of the modulation cylinder, the discharge port extends into the lower part of the mixing chamber, a solenoid valve air inlet is installed on the cylinder cover plate, a water injection pipe is connected to the surface of the cylinder cover plate, a deionized water injection pipe is connected to the surface of the cylinder cover plate, and a plurality of raw material injection pipes are connected to the surface of the cylinder cover plate; a water pumping port is opened inside the modulation cylinder, the water pumping port is connected to a liquid pumping pump, the liquid pumping pump is arranged on the outer wall of the modulation cylinder, and a helically coiled electric heating pipe is also arranged inside the modulation cylinder.

[0014] As a preferred technical solution of the present invention, a second servo motor is fixedly installed at the top of the cylinder cover plate. The second servo motor extends downward with a second rotating shaft. The second rotating shaft of the second servo motor extends into the bottom end of the cylinder cover plate, and an emulsion spreading plate is arranged at the bottom of the second rotating shaft extending into the bottom end of the cylinder cover plate.

[0015] As a preferred technical solution of the present invention, the diameter of the emulsion spreading plate rotating one week is located below several raw material injection pipes. An arc-shaped concave pit surface is arranged on the surface of the emulsion spreading plate, and the surface of the emulsion spreading plate is wavy.

[0016] As a preferred technical solution of the present invention, a third servo motor is fixedly installed at the top of each cylinder cover plate. The third servo motor extends downward with a rotating shaft. The rotating shaft of the third servo motor extends into the bottom end of the cylinder cover plate. Two or three water splashing paddle blades are arranged on the outer wall of the rotating shaft extending into the bottom end of the cylinder cover plate at equal circumferential intervals, and a water dripping port is arranged between adjacent two water splashing paddle blades.

[0017] As a preferred technical solution of the present invention, each water splashing paddle blade is an arc-shaped concave structure towards the rotation direction.

[0018] As a preferred technical solution of the present invention, the water pumping port includes a gate seal groove opened at the front end of the water pumping port. A replaceable liquid discharge filter element is arranged between the gate seal groove and the inner wall of the mixing cavity, and the liquid discharge filter element is detachable at the bottom of the modulation cylinder.

[0019] As a preferred technical solution of the present invention, the water pumping port is arranged in a square hole structure. A locking gate is slidably connected in the gate seal groove at the front end of the water pumping port. A spring groove is opened on one side wall of the gate seal groove. One end of the locking gate extends into the spring groove. A spring is arranged on the surface of the locking gate extending into the spring groove. An electromagnetic valve is fixedly installed on the surface of the spring groove in the sliding opening direction of the locking gate.

[0020] As a preferred technical solution of the present invention, the liquid discharge filter element is a metal filter element with tiny mesh holes on the surface. Scraper teeth with a triangular tooth structure are arranged on the surface of the locking gate towards the liquid discharge filter element.

[0021] As a preferred technical solution of the present invention, a lifting frame standing upright on the top end of the cylinder cover plate is fixedly installed at the top end of the cylinder cover plate. A slide rail is slidably connected to the surface of the lifting frame. A servo motor I is fixed to the surface of the slide rail. The top end of the stirring rod slidably extends out of the top end of the cylinder cover plate. The stirring rod extending out of the top end of the cylinder cover plate is fixedly connected to the output shaft of the servo motor I. An electric push rod is fixedly installed at the top end of the cylinder cover plate. The electric push rod extends upward with a push rod. The top end of the push rod of the electric push rod is fixed to the surface of the slide rail.

[0022] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0023] 1. In the preparation process of the present invention, steps S1 - S6 are all completed in the same stainless - steel cylinder. Therefore, the stainless - steel cylinder is the core technical content of the present invention. This stainless - steel cylinder (the modulation cylinder adopts a fully automatic batch - type multi - functional cylinder, which can integrate functions such as water washing, suction filtration, mixing, drying, self - heating, and self - cleaning in one mixing device; it has a small structural volume, can be used for multiple purposes, and has powerful functions. By automatically putting lignin and various raw materials for modification into the modulation cylinder in sequence according to the preparation steps, all processes of lignin preparation can be completed automatically. The modulation cylinder occupies a small area, and the batch - type treatment can automatically clean the inside of the mixing cavity after a batch of lignin is prepared, ensuring that the next batch of products is not contaminated.

[0024] 2. In the present invention, an emulsifier is added in step S3 first, and a liquid wax is added in the subsequent step S4. The effect is that the emulsifier makes lignin in a temporarily stable suspension state in the solvent, and then the liquid wax is used as a modifier to wrap the lignin particles to prevent the adhesion of the lignin emulsion. Moreover, if there is any remaining liquid wax, it can also play a lubricating and anti - aging role when the modified lignin is applied to rubber (anti - aging role: the wax swims to the surface of the rubber product during rubber vulcanization to form a protective layer); during the drying process, the particulate wax wraps the lignin to form particulate powder. When the modified lignin rubber is applied, with the dispersion effect of the wax, lignin can also be fully dispersed in the rubber matrix.

[0025] 3. The present invention has a mixing chamber inside the modulation cylinder, and a cylinder cover plate is installed at the top of the modulation cylinder. The locking and fixing between the cylinder cover plate and the modulation cylinder form a sealed connection. The airtight tank of ANFD can prevent toxic substances from polluting the air and also prevent external environment from polluting the lignin preparation process. In the middle of the bottom end of the cylinder cover plate, there is a stirring rod that rotates. At the bottom end of the stirring rod, there is a lifting paddle. The lignin to be processed is pressed into the mixing chamber through the feed pipe, and an appropriate amount of deionized water is injected into the mixing chamber through the deionized water injection pipe. Then, the lifting paddle continuously reciprocates up and down in the mixing chamber, and by the reciprocating flow of deionized water in the mixing chamber, the lignin is repeatedly rinsed to fully wash the lignin particles. After the rinsing is completed, the deionized water in the mixing chamber is suction-filtered through the bottom drainage filter element and the water suction port. During the suction filtration process, the lifting paddle keeps rotating, so that the water mixed on the surface of the lignin particles after water washing sinks down, and through the rotation of the lifting paddle on the inner bottom surface of the mixing chamber, the water liquid is deflected into the water suction port to improve the effect of suction-filtering water. During suction filtration, the solenoid valve air inlet on the cylinder cover plate is opened, and air enters the mixing chamber. By this method, repeated suction filtration can be achieved 4 - 5 times. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The present invention will be further described below in conjunction with the drawings and embodiments.

[0027] Figure 1 It is a flowchart of the steps of the method for preparing the emulsion of highly dispersed modified lignin of the present invention;

[0028] Figure 2 It is a front - view sectional view of the device for preparing the emulsion of highly dispersed modified lignin of the present invention;

[0029] Figure 3 It is a front - view structure diagram of the device for preparing the emulsion of highly dispersed modified lignin of the present invention;

[0030] Figure 4 It is a top - view structure schematic diagram of the emulsion spreading plate of the present invention;

[0031] Figure 5 It is a top - view sectional structure schematic diagram of the modulation cylinder of the present invention;

[0032] Figure 6 For the attached Figure 5 enlarged structure schematic diagram at location A of the specification of the present invention;

[0033] Figure 7 It is a bottom - view structure schematic diagram of the cylinder cover plate of the present invention;

[0034] Figure 8 It is a bottom - view structure schematic diagram of the water - splashing paddle of the present invention;

[0035] Figure 9Front view structural schematic diagram of the water - splashing blade of the present invention;

[0036] In the figure: modulation cylinder 1, support leg 2, electric heating tube 3, discharge port 4, feed pipe 5, locking screw 6, solenoid valve air inlet 7, electric push rod 8, lifting frame 9, slide rail 10, servo motor 1 11, raw material injection pipe 12, cylinder cover plate 13, servo motor 2 14, emulsion equalizing plate 15, stirring rod 16, lifting paddle blade 17, liquid discharge filter element 18, liquid extraction pump 19, sampling valve 20, rotating shaft 2 21, water injection pipe 22, gate seal groove 23, water extraction port 24, mixing cavity 25, tension spring groove 26, tension spring 27, solenoid valve 28, locking gate 29, chip scraping tooth 30, water - splashing blade 31, servo motor 3 32, deionized water injection pipe 33, concave pit surface 34, drip port 35, rotating shaft 36, vacuum tube 37. Specific implementation mode

[0037] In order to make the technical means, creative features, achieved purposes and effects of the present invention easy to understand, the following combines specific illustrations to further elaborate the present invention. It should be noted that, without conflict, the embodiments in this application and the features in the embodiments can be combined with each other.

[0038] Embodiment 1

[0039] Please refer to Figure 1 , which is the overall structural schematic diagram of a preparation method for a highly - dispersed modified lignin emulsion. A preparation method for a highly - dispersed modified lignin emulsion mainly includes the following steps:

[0040] S1. Wash lignin: Pour lignin into a stainless - steel cylinder, then add deionized water into the stainless - steel cylinder, soak lignin with deionized water and stir - wash it, then filter by suction to remove deionized water. After repeating the suction filtration 3 - 5 times, keep the washed lignin in the stainless - steel cylinder;

[0041] S2. Make dispersion liquid: Add an aqueous solution to the lignin retained in the stainless - steel cylinder to prepare a lignin dispersion liquid with a certain mass concentration, and control the pH value of the lignin dispersion liquid to be 7 - 8;

[0042] Specifically, in this embodiment, weigh a sufficient amount of lignin, add it into a stainless - steel cylinder, add deionized water and disperse it evenly, then filter by suction and wash it. Repeat 3 - 5 times to ensure that the lignin is washed clean. The inorganic salt content in the lignin is 0.01%, and the pH value is 6.5; Weigh 100 g of dry weight of the washed lignin and add it to a reaction kettle, add deionized water to prepare a lignin dispersion liquid with a mass concentration of 10%, and then adjust the pH value of the lignin dispersion liquid to 7; Stirring is carried out using a lifting paddle blade at a rotation speed of 50 r / min;

[0043] S3. Heating and emulsifying: Heat the bottom of the stainless - steel cylinder to a certain temperature, and then continuously stir the lignin dispersion liquid in the stainless - steel cylinder. During the stirring process, uniformly drip the emulsifier and emulsion stabilizer into the stainless - steel cylinder, and maintain the stirring speed during the dripping process;

[0044] Specifically, in this embodiment, the temperature is raised to 60 °C, and at the same time, the stirring speed is adjusted to 60 r / min. After the temperature is stable, start to drip 3 g of sodium fatty acid, 0.5 g of MOA7, and 0.5 g of AE02. After the dripping is completed, continue to stir for 1.5 h;

[0045] S4. Heating and injecting liquid wax: Continue to heat the bottom of the stainless - steel cylinder to increase the temperature inside the stainless - steel cylinder. During the process of temperature increase, synchronously increase the stirring speed of the lignin dispersion liquid inside the stainless - steel cylinder and maintain for a certain time to obtain an emulsion of highly dispersed modified lignin;

[0046] Specifically, in this embodiment, the temperature is raised to 80 °C, and the stirring rate is increased to 70 r / min. After the temperature is stable, slowly add 7 g of liquid wax to the emulsion. After the addition is completed, stir again for 1 h;

[0047] S5. Drying to obtain powder: Dry - process the emulsion inside the stainless - steel cylinder by heat - drying. During the drying process, continuously stir the inside of the stainless - steel cylinder to obtain highly dispersed modified lignin particle powder;

[0048] S6. Discharging and cooling: Discharge the obtained highly dispersed modified lignin particle powder from the inside of the stainless - steel cylinder, and then quickly cool it to normal temperature (below 25 °C), then the production and preparation of highly dispersed modified lignin can be completed.

[0049] Specifically, in this embodiment, after heat - drying treatment, a powder with a moisture content ≤ 5% is obtained, and the obtained powder is discharged from the inside of the stainless - steel cylinder and quickly cooled to normal temperature (25 °C) or below.

[0050] Specifically, in this embodiment, the present invention first adds an emulsifier in step S3 and adds liquid wax in the subsequent step S4. The effect is that the emulsifier makes lignin in a temporarily stable suspension state in the solvent, and then liquid wax is used as a modifier to wrap lignin particles to prevent the adhesion of lignin emulsion. Moreover, if there is remaining liquid wax, it can also play a lubricating and anti - aging role when the modified lignin is applied to rubber (anti - aging role: the wax migrates to the surface of the rubber product during rubber vulcanization to form a protective layer); during the drying process, the particulate wax wraps the lignin to form particulate powder. When the modified lignin rubber is applied, with the dispersion effect of the wax, lignin can also be fully dispersed in the rubber matrix.

[0051] Example 2

[0052] Please refer toFigures 2 - 9 , this embodiment has similarities with the above-mentioned Embodiment 1, and the similarities will not be elaborated in this embodiment. The specific differences are as follows:

[0053] According to the method for preparing an emulsion of highly dispersed modified lignin described in the above-mentioned Embodiment 1, this embodiment also provides a device for preparing an emulsion of highly dispersed modified lignin to cooperate. The device for preparing an emulsion of highly dispersed modified lignin includes a modulation cylinder 1. The modulation cylinder 1 is set as a cylindrical structure. Inside the modulation cylinder 1, there is a mixing chamber 25. At the top of the modulation cylinder 1, there is a cylinder cover plate 13. In the middle of the bottom end of the cylinder cover plate 13, there is a rotating stirring rod 16. At the bottom end of the stirring rod 16, there is a lifting paddle 17. The outer wall of the modulation cylinder 1 is connected with a feed pipe 5, and the feed pipe 5 extends into the upper part of the mixing chamber 25. The outer wall of the modulation cylinder 1 is connected with a discharge port 4, and the discharge port 4 extends into the lower part of the mixing chamber 25. The cylinder cover plate 13 is equipped with a solenoid valve air inlet 7. The surface of the cylinder cover plate 13 is connected with a water injection pipe 22, the surface of the cylinder cover plate 13 is connected with a deionized water injection pipe 33, and the surface of the cylinder cover plate 13 is connected with a plurality of raw material injection pipes 12. Inside the modulation cylinder 1, there is a water extraction port 24, and the water extraction port 24 is connected to a liquid extraction pump 19. The liquid extraction pump 19 is arranged on the outer wall of the modulation cylinder 1. Inside the modulation cylinder 1, there is also a spirally coiled electric heating pipe 3.

[0054] Specifically, in this embodiment, first, steps S1 - S6 in the preparation process of the present invention are all completed in the same stainless steel cylinder. Therefore, the stainless steel cylinder is the core technical content of the present invention. This stainless steel cylinder (the modulation cylinder 1) is a fully automatic batch - type multi - functional cylinder, which can integrate functions such as water washing, suction filtration, mixing, drying, self - heating, and self - cleaning in one mixing device; it has a small structural volume, can be used for multiple purposes, and has powerful functions. By automatically putting lignin and various raw materials for modification into the modulation cylinder 1 in sequence according to the preparation steps, all processes of lignin preparation can be completed automatically. The modulation cylinder 1 occupies a small area, and the batch - type processing can automatically clean the inside of the mixing chamber 25 after preparing a batch of lignin, ensuring that the next batch of products is not contaminated.

[0055] Specifically, in this embodiment, the present invention is provided with a mixing chamber 25 inside the modulation cylinder 1. A cylinder cover plate 13 is installed at the top of the modulation cylinder 1. The locking and fixing between the cylinder cover plate 13 and the modulation cylinder 1 form a sealed connection. The airtight tank body of ANFD can avoid the pollution of toxic substances to the air and also avoid the pollution of the external environment to the lignin preparation process. In the middle of the bottom end of the cylinder cover plate 13, there is a stirring rod 16 that rotates. At the bottom end of the stirring rod 16, there is a lifting paddle 17. The lignin to be processed is pressed into the mixing chamber 25 through the feed pipe 5. An appropriate amount of deionized water is injected into the mixing chamber 25 through the deionized water injection pipe 33. Then, the lifting paddle 17 continuously reciprocates up and down in the mixing chamber 25. By using the reciprocating flow of deionized water in the mixing chamber 25, the lignin is repeatedly rinsed to fully wash the lignin particles. After the rinsing is completed, the deionized water in the mixing chamber 25 is filtered by the bottom drainage filter element 18 and the water pumping port 24. During the filtration process, the lifting paddle 17 keeps rotating, so that the water mixed on the surface of the washed lignin particles sags and sinks. Through the rotation of the lifting paddle 17 on the inner bottom surface of the mixing chamber 25, the water liquid is deflected into the water pumping port 24, improving the effect of filtering water. During filtration, the air inlet 7 of the solenoid valve 28 on the cylinder cover plate 13 is opened, and air enters the mixing chamber 25. By this method, repeated filtration can be achieved 4 - 5 times.

[0056] Specifically, in this embodiment, the present invention heats the inner wall of the mixing chamber 25 through the electric heating tube 3. The electric heating tube 3 has high heating efficiency and simple temperature control. It can quickly heat up when dropping liquid wax, preventing the liquid wax from condensing during the dropping process. At the same time, during the later hot drying process, the emulsion in the mixing chamber 25 is heated by the electric heating tube 3. Cooperating with the vacuum extraction inside the mixing chamber 25 can reduce the system pressure, thereby reducing the boiling point of the liquid, achieving a faster drying speed. In addition, the reduction of the boiling point can also avoid the occurrence of high-temperature decomposition reactions, and the liquid in the powder can evaporate more quickly, thus achieving the purpose of rapid drying. During this period, the sampling valve 20 can be used for on-line sampling to analyze the moisture content of the filter cake to meet the requirements of controlling product quality.

[0057] A servo motor two 14 is fixedly installed at the top end of the cylinder cover plate 13. The servo motor two 14 extends downward with a rotating shaft two 21. The rotating shaft two 21 of the servo motor two 14 extends into the bottom end of the cylinder cover plate 13, and at the bottom of the rotating shaft two 21 extending into the bottom end of the cylinder cover plate 13, there is an emulsion spreading plate 15.

[0058] The diameter of the emulsion spreading plate 15 rotating one week is located below several raw material injection pipes 12. There are concave pits 34 with arc-shaped depressions on the surface of the emulsion spreading plate 15, and the surface of the emulsion spreading plate 15 is wavy.

[0059] Specifically, in this embodiment, after the water washing of the present invention is completed, an appropriate amount of water is injected into the mixing chamber 25 through the water injection pipe 22 at the top of the cylinder cover plate 13, and a dispersion liquid is prepared by rotating and stirring in the mixing chamber 25 with the lifting paddle 17. During the rotation and stirring process, the inner wall of the mixing chamber 25 is heated by the electric heating tube 3 to increase the temperature of the inner wall of the mixing chamber 25, which is convenient for increasing the activity of the dispersion liquid. At the same time, the diameter of the emulsion spreading plate 15 rotating one week is located below several raw material injection pipes 12, and emulsifiers and emulsion stabilizing agents of multiple different raw materials are simultaneously added to the dispersion liquid in the mixing chamber 25 through the several raw material injection pipes 12. During the dropping process, the emulsion spreading plate 15 rotates to evenly mix and sprinkle the emulsifiers and emulsion stabilizing agents dropped from the several raw material injection pipes 12. When the emulsifiers and emulsion stabilizing agents drip downward from the several raw material injection pipes 12, a part of them is received by the concave surface 34 on the surface of the emulsion spreading plate 15. Different emulsifiers and different emulsion stabilizing agents dripping on the concave surface 34 fall vertically under the action of gravity and collide and locally disperse during the falling process, so as to achieve preliminary uniform mixing in the concave surface 34 and are thrown out by the rotation of the emulsion spreading plate 15, so that a part of the emulsifiers and emulsion stabilizing agents dripping downward from the several raw material injection pipes 12 vertically fall into the lower mixing chamber 25, and a part of the emulsifiers and emulsion stabilizing agents that are preliminarily mixed are rotated and thrown out by the emulsion spreading plate 15 to the area where it is not easy to mix at the inner wall edge of the mixing chamber 25, which is beneficial to improving the mixing uniformity of the emulsifier and the dispersion liquid and increasing the component uniformity of the modified lignin emulsion particles.

[0060] A servo motor three 32 is fixedly installed at the top of each cylinder cover plate 13. A rotating shaft 36 extends downward from the servo motor three 32. The rotating shaft 36 of the servo motor three 32 extends into the bottom end of the cylinder cover plate 13. Two or three water splashing paddles 31 are arranged on the outer wall of the rotating shaft 36 extending into the bottom end of the cylinder cover plate 13 at equal circumferential intervals, and a water dripping port 35 is arranged between adjacent two water splashing paddles 31.

[0061] The orientation of each water splashing paddle 31 in the rotation direction is an arc-shaped concave structure, similar to a hand-holding shape.

[0062] Specifically, in this embodiment, inside the mixing chamber 25 after hot drying, the lifting paddle 17 rotates reciprocally to push the modified lignin particles out from the discharge port 4. After the discharge, water is injected into the mixing chamber 25 through the water injection pipe 22 above to clean the inside of the mixing chamber 25. During the water injection process, the water splashing paddle 31 located below the water injection pipe 22 rotates. There are two or three water splashing paddles 31 arranged at equal intervals in a circular pattern on the outer wall of the rotating shaft 36. A water dripping opening 35 is provided between two adjacent water splashing paddles 31. Then, part of the water liquid injected from the water injection port vertically drips downward into the mixing chamber 25 through the water dripping opening 35, and part of it falls on the rotating water splashing paddle 31. Each water splashing paddle 31 has an arc-shaped concave structure facing the rotation direction, similar to the action of a palm holding water, which holds the water liquid and splashes it on the inner wall surface of the mixing chamber 25, thereby splashing and washing the inner wall of the warm material chamber. At the same time, due to the arc-shaped concave structure of the water splashing paddle 31, the water liquid can be splashed to a higher position on the inner wall of the mixing chamber 25. Thus, when the lifting paddle 17 cannot stir and clean to a higher position, it can be cleaned thoroughly through splashing and washing, so as to realize the internal cleaning of the container environment and ensure that the next batch of products is not contaminated.

[0063] The water pumping port 24 includes a gate seal groove 23 opened at the front end of the water pumping port 24. A replaceable drainage filter element 18 is arranged between the gate seal groove 23 and the inner wall of the mixing chamber 25. The drainage filter element 18 is detachable at the bottom of the modulation cylinder 1, which is convenient for later replacement.

[0064] The water pumping port 24 is set as a square hole structure. A locking gate 29 is slidably connected in the gate seal groove 23 at the front end of the water pumping port 24. A tension spring groove 26 is opened on one side wall of the gate seal groove 23. One end of the locking gate 29 extends into the tension spring groove 26. A tension spring 27 is arranged on the surface of the locking gate 29 extending into the tension spring groove 26. An electromagnetic valve 28 is fixedly installed on the surface of the tension spring groove 26 in the sliding opening direction of the locking gate 29.

[0065] The drainage filter element 18 is a metal filter element with tiny mesh holes on the surface. Scraper teeth 30 with a triangular tooth structure are opened on the surface of the locking gate 29 facing the drainage filter element 18.

[0066] Specifically, in this embodiment, the water intake 24 of the present invention includes a gate seal groove 23 opened at the front end of the water intake 24. A replaceable drain filter element 18 is arranged between the gate seal groove 23 and the inner wall of the mixing chamber 25. The drain filter element 18 is detachable at the bottom of the modulation cylinder 1, which is convenient for later maintenance, cleaning or replacement. The water intake 24 is set as a square hole structure. A locking gate 29 is slidably connected in the gate seal groove 23 at the front end of the water intake 24. The water intake 24 is automatically opened or closed and sealed through the locking gate 29, so that the water intake 24 can be effectively opened and closed automatically. A spring 27 groove 26 is opened on one side wall of the gate seal groove 23. One end of the locking gate 29 extends into the spring 27 groove 26. A spring 27 is arranged on the surface of the locking gate 29 extending into the spring 27 groove 26. An electromagnetic valve 28 is fixedly installed on the surface of the spring 27 groove 26 in the sliding opening direction of the locking gate 29. The electromagnetic valve 28 is used to realize that the locking gate 29 is in a short-term opening and long-closed state. When the electromagnetic valve 28 is energized, a magnetic attraction is generated to lock the gate 29 to slide along the gate seal groove 23 to open the water intake 24. When the electromagnetic valve 28 is de-energized, the locking gate 29 is pulled by the spring 27 to slide along the gate seal groove 23 to the position where the water intake 24 is closed. At the same time, during the reciprocating sliding of the locking gate 29, the scraping teeth 30 of the triangular tooth structure on the surface of the locking gate 29 scrape the surface of the drain filter element 18, so as to effectively prevent the surface of the drain filter element 18 from being blocked, thereby improving the fluidity of the filtered water.

[0067] At the top end of the cylinder cover plate 13, a lifting frame 9 standing upright at the top end of the cylinder cover plate 13 is fixedly installed. A slide rail 10 is slidably connected to the surface of the lifting frame 9. A servo motor 11 is fixed on the surface of the slide rail 10. The top end of the stirring rod 16 slides out of the top end of the cylinder cover plate 13. The stirring rod 16 extending out of the top end of the cylinder cover plate 13 is fixedly connected to the output shaft of the servo motor 11. An electric push rod 8 is fixedly installed at the top end of the cylinder cover plate 13. The electric push rod 8 extends upward with a push rod. The top end of the push rod of the electric push rod 8 is fixed on the surface of the slide rail 10, which is convenient for driving the lifting paddle to reciprocate up and down in the mixing chamber 25.

[0068] Among them, in this embodiment, a sealing structure is adopted for the connection between the stirring rod 16 and the cylinder cover plate 13. This connection method is an existing technology, and the specific connection method is not the technical content of the present invention. Therefore, the specific structure is not described in this embodiment. Any technology in the existing technology as long as it achieves the technical effects described in this application can be used as a substitute for the present invention.

[0069] Among them, in this embodiment, independent solenoid valves are provided in the middle of pipelines such as the discharging port 4, the feeding pipe 5, the raw material injection pipe 12, the sampling valve 20, the water injection pipe 22, and the deionized water injection pipe 33 to control the on-off. In addition, a vacuum pipe 37 for extracting the vacuum inside the mixing chamber is connected to the surface of the cylinder cover plate 13. The position of the vacuum pipe 37 can be set at any position on the surface of the cylinder cover plate 13, which is convenient for vacuum extraction during the hot drying process and will not be elaborated in this embodiment.

[0070] In this embodiment, support legs 2 are provided at the bottom of the modulation cylinder 1 to facilitate supporting the modulation cylinder 1 and making the placement of the modulation cylinder 1 more stable.

[0071] In this embodiment, a plurality of locking screws 6 are connected between the top end of the modulation cylinder 1 and the cylinder cover plate 13. The cylinder cover plate 13 is locked and fixed to the top end of the modulation cylinder 1 through the plurality of locking screws 6, and the locking firmness of the cylinder cover plate 13 and the sealing firmness are improved by the locking screws 6.

[0072] The above shows and describes the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The descriptions in the above embodiments and the specification only illustrate the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements fall within the scope of the present invention claimed. The scope of protection claimed by the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing an emulsion of highly dispersed modified lignin, characterized in that, The method for preparing the emulsion of highly dispersed modified lignin mainly includes the following steps: S1. Washing lignin: Pour lignin into a stainless-steel cylinder, then add deionized water into the stainless-steel cylinder, soak lignin with deionized water and stir and wash it, then filter to remove deionized water. After filtering repeatedly for 3 - 5 times, keep the washed lignin in the stainless-steel cylinder; S2. Preparing the dispersion liquid: Add aqueous solution to the lignin retained in the stainless-steel cylinder to obtain a lignin dispersion liquid with a certain mass concentration, and control the pH value of the lignin dispersion liquid to be 7 - 8; S3. Heating and emulsifying: Heat the bottom of the stainless-steel cylinder to a certain temperature, then continuously stir the lignin dispersion liquid in the stainless-steel cylinder. During the stirring process, evenly drop the emulsifier and emulsification stabilizer into the stainless-steel cylinder, and keep the stirring speed during the dropping process; S4. Raising the temperature and injecting liquid wax: Continue to heat the bottom of the stainless-steel cylinder to increase the temperature inside the stainless-steel cylinder. During the process of temperature increase, synchronously accelerate the stirring speed of the lignin dispersion liquid inside the stainless-steel cylinder and keep it for a certain time to obtain the emulsion of highly dispersed modified lignin; S5. Drying to obtain powder: Dry the emulsion inside the stainless-steel cylinder by thermal drying method. During the drying process, continuously stir the inside of the stainless-steel cylinder to obtain the granular powder of highly dispersed modified lignin; S6. Discharging and cooling: Discharge the obtained granular powder of highly dispersed modified lignin from the inside of the stainless-steel cylinder, and then quickly cool it to room temperature (below 25°C), then the production and preparation of highly dispersed modified lignin can be completed.

2. The method for preparing an emulsion of highly dispersed modified lignin according to claim 1, wherein: The above-mentioned steps S1 - S5 are mainly completed in cooperation with a device for preparing the emulsion of highly dispersed modified lignin. The device for preparing the emulsion of highly dispersed modified lignin includes a modulation cylinder. The modulation cylinder is set as a cylindrical structure. There is a mixing chamber inside the modulation cylinder. A cylinder cover plate is installed at the top of the modulation cylinder. In the middle of the bottom end of the cylinder cover plate, there is a stirring rod that rotates and turns. At the bottom end of the stirring rod, there is a lifting paddle. The outer wall of the modulation cylinder is connected with a feed pipe, and the feed pipe extends into the upper part of the mixing chamber. The outer wall of the modulation cylinder is connected with a discharge port, and the discharge port extends into the lower part of the mixing chamber. The cylinder cover plate is equipped with a solenoid valve air inlet. The surface of the cylinder cover plate is connected with a water injection pipe, a deionized water injection pipe, and several raw material injection pipes; There is a water pumping port opened inside the modulation cylinder, and the water pumping port is connected to a liquid pumping pump. The liquid pumping pump is arranged on the outer wall of the modulation cylinder. Inside the modulation cylinder, there is also a helically coiled electric heating pipe.

3. The emulsion preparation method of a highly dispersed modified lignin according to claim 2, characterized in that: A servo motor two is fixedly installed at the top end of the cylinder cover plate. The servo motor two extends downward with a rotating shaft two. The rotating shaft two of the servo motor two extends into the bottom end of the cylinder cover plate. At the bottom of the rotating shaft two extending into the bottom end of the cylinder cover plate, there is an emulsion spreading plate.

4. The method for preparing an emulsion of highly dispersed modified lignin according to claim 3, wherein: The diameter of one rotation of the emulsion spreading plate is located below several raw material injection pipes. There is an arc-shaped sunken pit surface in the middle of the surface of the emulsion spreading plate, and the surface of the emulsion spreading plate is in a wavy shape.

5. The emulsion preparation method of a highly dispersed modified lignin according to claim 2, wherein: A servo motor three is fixedly installed at the top of each of the cylinder cover plates. The servo motor three extends downward with a rotating shaft. The rotating shaft of the servo motor three extends into the bottom end of the cylinder cover plate. Two or three water splashing blades are arranged on the outer wall of the rotating shaft extending into the bottom end of the cylinder cover plate at equal circumferential intervals. A water dripping port is arranged between adjacent two of the water splashing blades.

6. The emulsion preparation method of a highly dispersed modified lignin according to claim 5, characterized in that: Each of the water splashing blades is an arc-shaped concave structure facing the rotation direction.

7. The emulsion preparation method of a highly dispersed modified lignin according to claim 2, characterized in that: The water pumping port includes a gate seal groove opened at the front end of the water pumping port. A replaceable liquid discharge filter element is arranged between the gate seal groove and the inner wall of the mixing chamber. The liquid discharge filter element is detachable at the bottom of the modulation cylinder.

8. The emulsion preparation method of a highly dispersed modified lignin according to claim 7, characterized in that: The water pumping port is arranged in a square hole structure. A locking gate is slidably connected in the gate seal groove at the front end of the water pumping port. A tension spring groove is opened on one side wall of the gate seal groove. One end of the locking gate extends into the tension spring groove. A tension spring is arranged on the surface of the locking gate extending into the tension spring groove. An electromagnetic valve is fixedly installed on the surface of the tension spring groove located in the sliding opening direction of the locking gate.

9. The method for preparing an emulsion of a highly dispersed modified lignin according to claim 8, characterized in that: The liquid discharge filter element is a metal filter element with tiny mesh holes on the surface. Scraping teeth with a triangular tooth structure are arranged on the surface of the locking gate facing the liquid discharge filter element.

10. The method for preparing an emulsion of highly dispersed modified lignin according to claim 2, characterized in that: A lifting frame standing upright at the top of the cylinder cover plate is fixedly installed at the top of the cylinder cover plate. A slide rail is slidably connected to the surface of the lifting frame. A servo motor one is fixed on the surface of the slide rail. The top end of the stirring rod slides out of the top of the cylinder cover plate. The stirring rod extending out of the top of the cylinder cover plate is fixedly connected to the output shaft of the servo motor one. An electric push rod is fixedly installed at the top of the cylinder cover plate. The electric push rod extends upward with a push rod. The top end of the push rod of the electric push rod is fixed to the surface of the slide rail.

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