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WO2021051780A1 - Procédé de préparation de fibre fonctionnalisée superfine à l'aide de drêches de distillerie - Google Patents

Procédé de préparation de fibre fonctionnalisée superfine à l'aide de drêches de distillerie Download PDF

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Publication number
WO2021051780A1
WO2021051780A1 PCT/CN2020/082853 CN2020082853W WO2021051780A1 WO 2021051780 A1 WO2021051780 A1 WO 2021051780A1 CN 2020082853 W CN2020082853 W CN 2020082853W WO 2021051780 A1 WO2021051780 A1 WO 2021051780A1
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WO
WIPO (PCT)
Prior art keywords
fiber
screen
distiller
reaction
grains
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2020/082853
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English (en)
Chinese (zh)
Inventor
王俊祥
吕宪俊
陈平
曹晓强
李琳
冯艳斐
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Shandong University of Science and Technology
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Shandong University of Science and Technology
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Application filed by Shandong University of Science and Technology filed Critical Shandong University of Science and Technology
Priority to RU2021108113A priority Critical patent/RU2764132C1/ru
Publication of WO2021051780A1 publication Critical patent/WO2021051780A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/123—Ultraviolet light
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/126—Microwaves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/001—Treatment with visible light, infrared or ultraviolet, X-rays
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/003—Treatment with radio-waves or microwaves
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/06—Inorganic compounds or elements
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08—Organic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • D06M13/5135—Unsaturated compounds containing silicon atoms
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres

Definitions

  • the present invention relates to the field of distiller's grains processing, in particular to a process for extracting grain fibers from distiller's grains and performing functional modification to prepare ultra-fine functionalized fibers. Background technique
  • Distiller's grains are solid by-products produced by the winemaking and alcohol industry. They are rich in fiber, amino acids, crude starch, various enzymes and vitamins, and have the characteristics of large yield, complex components, and poor storage stability. Distillers' grains can be roughly divided into beer's grains, white wine's grains, rice wine's grains, and alcohol's grains.
  • distiller’s grains With the increase in the industrialization of wine and alcohol industries, the output of distiller’s grains is increasing day by day. With the enhancement of social environmental protection awareness and the development of science and technology, enterprises can no longer simply use distiller’s grains as waste and directly landfill it as before. How to reasonably and efficiently use distiller’s grains has become a problem that plagues enterprises and related scientific researchers
  • the invention patent with application number 201711210006.1 discloses a method for preparing a culture medium using distiller's grains as the main raw material, which is simple in process and convenient to use.
  • the application number is 201910627735.
  • X’s invention patent discloses a method for preparing flavored wine using distiller’s lees. Through pretreatment, enzymolysis, fermentation, and blending, the effective ingredients in distiller’s lees are fully utilized and the environmental pollution of distiller’s lees is reduced. .
  • the invention patent with the application number 201910627741. 5 discloses a method for extracting dietary fiber from distiller’s lees. Through a series of processes such as refining and enzymatic hydrolysis, the extraction of dietary fiber from distiller’s lees is realized, which further improves the added value and utilization of distiller’s spent grain value.
  • the use of distiller's grains to make animal feed or fertilizer is also an important way to utilize distiller's grains.
  • the invention patent with application number 201510792499. 9 discloses a method for preparing cattle and sheep feed through sealed fermentation using distiller's grains, feed complex enzymes and feed prebiotics, which greatly reduces the production cost of feed.
  • the invention patent with application number 201810608098 discloses a method for extracting dietary fiber from distiller’s lees. Through a series of processes such as refining and enzymatic hydrolysis, the extraction of dietary fiber from distiller’s lees is realized, which further improves the added value and utilization of distill
  • the invention patent of 01711360873. 3 discloses a method for producing organic fertilizer with distiller’s grains, straw, superphosphate, etc. as the main raw materials.
  • the organic fertilizer is produced through the process of ingredient-prophase aerobic fermentation-late anaerobic fermentation-drying granulation. It has passed the certification of the National Green Food Development Center and is suitable for a variety of agricultural products such as corn, rice, cotton, and vegetables.
  • the invention patent with application number 201510656869. 6 discloses a method for modifying raw soil materials by using grain distiller’s lees.
  • the modified raw soil materials are prepared after mixing the distiller’s grains, raw soil and inorganic cementing materials in a certain proportion.
  • the plant fibers in the distiller’s grains are fully utilized, and the mechanical properties of the raw soil blocks are improved.
  • the purpose of the present invention is to propose a process for preparing ultra-fine functionalized fibers from distiller's grains, which provides a new feasible way for the efficient utilization of distiller's grains.
  • a process for preparing ultra-fine functionalized fibers from distiller’s grains includes the following steps:
  • Al distillers grains are transported to the distillers grain temporary storage box, and then fed into the shearing crusher under the action of the first electric vibrating feeder, and at the same time, they are sheared according to the weight ratio of distillers grain: water of 1:3 ⁇ 1:5. Add water to the crusher;
  • a2 Distillers grains are crushed in a shearing crusher, and then flow into the high-frequency vibrating fine sieve from the discharge port;
  • the fiber pre-disintegration reactor is a split structure, including a fixed reactor body and a detachable type
  • the reaction sieve is added with the fiber pre-decomposition liquid inside the fixed reaction kettle body, the fibers in the first fiber temporary storage tank are placed in a separable reaction sieve, and the separable reaction sieve is placed inside the fixed reaction kettle body, and then Immerse the fiber in the fiber pre-decomposition liquid;
  • the fiber pre-decomposition liquid consists of 1 to 5 parts of hydrogen peroxide, 0.5 to 3 parts of potassium persulfate, 0.2 to 2 parts of accelerator and 90 to 97.3 parts of water in parts by weight;
  • the accelerator is one or more of cobalt chloride, cobalt ammonia complex, ferrous chloride, and ferrous sulfate;
  • the mass ratio of the fiber to the fiber pre-decomposition liquid is 1: 3 to 1: 5
  • the reaction temperature during the fiber pre-decomposition is 30 to 85 ° C
  • sodium hydroxide is used to adjust the pH of the pre-decomposition liquid during the reaction 6 ⁇ 10
  • the reaction time is 0.5 ⁇ 4 hours
  • the detachable reaction sieve is lifted from the fixed reactor body by the hook on the circulating chain conveyor. During the transportation process, gravity and the sieve barrier effect of the detachable reaction sieve are used to realize the fiber Separation from the pre-decomposition liquid;
  • the pre-decomposed fiber of dl is fed into the second fiber temporary storage tank, and then fed into the material conveying belt under the action of the third electric vibrating feeder, and two water washes are respectively arranged above the material conveying belt along the material conveying direction.
  • Device and two functional modifier spray devices used to wash materials and realize the modifier to fully wet the fibers;
  • the fiber After spraying the functional modifier, the fiber continues to be transported by the material conveying belt to the photocatalytic microwave synergistic reactor, and the functional modification of the fiber is performed under the combined action of a fixed wavelength light source and microwave to obtain ultra-fine functionalization. fiber.
  • flushing water is provided at the discharge port of the shearing crusher to ensure the smooth flow of materials after crushing; a valve is provided at the lower end of the shearing crusher to control the flow of materials and the shearing and crushing time of vinasse .
  • an under-screen material recovery tank is provided below the high-frequency vibrating fine screen, and the material in the under-screen material recovery tank is After the material is filtered or press-filtered, the filter cake is used as a fertilizer or a medium raw material, and the filtrate is returned to the high-speed shearing and pulverizing step of distiller's grains for reuse.
  • the fiber pre-disintegration reactor further includes a liftable stirring device and a reaction kettle cover
  • the liftable stirring device includes a stirring paddle, a stirring motor, a vertical fixed rod and a lifting adjustment device, and a lifting adjustment device cover
  • the lifting adjustment device is connected with the stirring motor through the horizontal support rod
  • the stirring motor is connected with the stirring paddle in transmission
  • the stirring paddle is arranged vertically;
  • the reactor cover is opened, the fiber pre-decomposition liquid is added to the reactor body, and the fibers are fed into the separable reaction sieve and then immersed in the fiber pre-decomposition liquid;
  • the paddle is lowered to a suitable height, and the fiber is pre-decomposed after closing the lid of the reactor.
  • the separable reaction sieve has a frame structure, specifically a square or cylindrical body, etc., the sieve body of the separable reaction sieve is surrounded by a sieve surface, and the bottom of the detachable reaction sieve is The movable screen, one end of the movable screen is hinged with the bottom of the screen surface through a hinge, the opening and closing of the movable screen is controlled by a mechanical switch, and the top of the detachable reaction screen is also provided with a hoisting ring that is convenient for lifting.
  • the mechanical switch is a spring-linked switch
  • the spring-linked switch includes a first link and a second link, the first link and the second link are both vertically arranged, and the first link is connected to the
  • the screen body is connected, the bottom of the first connecting rod is connected with the top of the second connecting rod through a spring, and the bottom of the second connecting rod is formed with a horizontal bending part for supporting the movable screen; the second connecting rod is rotated to cooperate with the control
  • the movable screen can be opened and closed.
  • the circulating chain conveying device includes a traction chain, a conveying track, and a hanging platform, the traction chain is connected with the conveying motor, the hanging platform is connected with the traction chain, and the hanging platform is mounted on the conveying track , The hanging platform is driven by the conveying motor through the traction chain to run along the conveying track, and a hook is provided at the bottom of the hanging platform;
  • the conveying track is undulating, and the detachable reaction screen is gradually moved under the traction of the traction chain, and vibrates continuously with the undulating conveying track, and realizes the fiber and the pre-decomposition liquid under the dual effects of vibration and gravity.
  • the rapid separation The beneficial effects of the invention
  • the present invention proposes a process for quickly extracting fiber components from distiller’s grains, and using different types of modifiers to perform functional modification on them according to uses; ultrafine functional fibers obtained after modification Can be used as The modification of concrete mortar and coating products provides a feasible way for the efficient utilization of distiller's lees, which can greatly improve the economic and utilization value of related products of distiller's lees.
  • the present invention divides fiber modification into two processes of pre-decomposition and functional modification. Under the action of the self-made pre-decomposition liquid, the fracture of the bridging oxygen bond in the fiber is quickly realized, and the subsequent modification active sites are increased. Quantity, greatly improve the fiber modification efficiency and degree of modification.
  • FIG. 1 is a schematic diagram of the process flow of the present invention
  • FIG. 2 is a side view of the separable reaction screen in the present invention, and the figure shows the state when the bottom movable screen is closed;
  • FIG. 3 is a side view of the separable reaction screen in the present invention, and the figure shows the state when the bottom movable screen is opened;
  • FIG. 4 is a schematic diagram of the structural principle of the fiber pre-disintegration reactor in the present invention, which shows the reaction state when the lid of the reactor is closed;
  • FIG. 5 is a schematic diagram of the structural principle of the fiber pre-disintegration reactor in the present invention, and the figure shows the feeding state when the lid of the kettle is opened;
  • FIG. 6 is a schematic diagram of the structure principle of the circulating chain conveying device in the present invention, and the figure shows a top view state;
  • FIG. 7 is a schematic diagram of the structural principle of the photocatalytic microwave synergistic reactor in the present invention.
  • 1-Temporary storage tank for distiller's grains 2-First electric vibration feeder; 3-High-speed shearing crusher; 4-High-frequency vibrating fine sieve; 5-Subsieve material recovery pool; 6-Flushing Water; 7-First fiber temporary storage tank; 8-Second electric vibrating feeder; 9-Fiber pre-disintegration reactor; 10- Fixed reactor body; 11- Separate reaction screen; 12-Liftable stirring Device; 13-Circulating chain conveying device; 14-Pre-decomposition liquid recovery tank; 15-Second fiber temporary storage tank; 16-The third electric vibrating feeder, 17-Material conveying belt; 18-Water washing device; 19-Functional modifier spraying device; 20-Photocatalytic microwave synergistic reactor; 21-Washing water recovery tank; 22 -Functionalized modifier recovery pool;
  • 11-1 the screen surface of the reaction sieve; 1-2: relatively chain; 11-3: movable sieve; 1-4: horizontal bending part; 11
  • 12-1 Lifting and adjusting device
  • 12-2 Vertical fixed rod
  • 12-3 Stirring paddle
  • 12-4 Stirring motor
  • 13-1 Conveying track
  • 13-2 Traction chain
  • 13-3 Hanging platform
  • 13-4 Conveying motor
  • a process for preparing ultra-fine functional fibers from distiller’s grains includes the following steps:
  • Al distillers grains do not need to be dried. After being conveyed to the distillers grain temporary storage box 1 through a belt, they are fed into the high-speed shearing crusher 3 under the action of the first electric vibrating feeder 2, and at the same time according to the distillers grain: water ratio of 1: 3 ⁇ Add water to the high-speed shearing crusher 3 with a weight ratio of 1:5.
  • a2 Distillers grains are crushed to a suitable level in the high-speed shearing crusher 3 by the high-speed dispersion of the shearing and crushing cutter Then it flows into the high frequency vibrating fine sieve 4 from the discharge port.
  • the discharge port of the high-speed shearing crusher 3 is provided with flushing water to ensure the smooth outflow of the material after crushing.
  • a valve is installed at the lower end of the high-speed shearing crusher to control the material flow and the vinasse shearing and crushing time.
  • b2 is provided with two washing water 6 above the high-frequency vibrating fine screen 4, respectively located in the middle and the end of the high-frequency vibrating fine screen, for washing the separated fiber components.
  • the material discharged from the high-speed shearing crusher 3 is directly fed into the high-frequency vibrating fine sieve 4 for the separation of fibers and other components in the distiller’s grains.
  • the high-frequency vibrating fine screen 4 has adjustable amplitude, inclination and frequency, and is used to control the separation speed and separation effect of materials.
  • the filter cake is used as a fertilizer or a medium raw material, and the filtrate is returned to the high-speed shearing and crushing step of distiller's grains for reuse, which can replace part of the water during high-speed shearing and crushing of distiller's grains the amount.
  • cl is fed to the first fiber temporary storage tank 7 by the fiber components separated from the high-frequency vibrating fine sieve 4 sieve.
  • the fiber pre-decomposing reactor 9 has a split structure, including a fixed reactor body 10 and a separable reaction screen 11.
  • the fiber pre-decomposition liquid is added to the fixed reactor body 10, and the first fiber temporary storage tank 7
  • the fiber is placed in the detachable reaction sieve 11, and the detachable reaction sieve 11 is placed inside the fixed reactor body 10, so that the fibers are immersed in the fiber pre-decomposition liquid.
  • the fiber pre-decomposition liquid consists of 1 to 5 parts by weight of hydrogen peroxide (30%), 0.5 to 3 parts of potassium persulfate, 0
  • the accelerator is one or more complexes of cobalt chloride, cobalt ammonia complex, ferrous chloride, and ferrous sulfate.
  • the mass ratio of the fiber to the fiber pre-decomposition liquid is 1: 3 to 1: 5
  • the reaction temperature during the fiber pre-decomposition is 30 to 85 ° C
  • sodium hydroxide is used to adjust the pH of the pre-decomposition liquid during the reaction 6 ⁇ 10
  • the reaction time is 0.5 ⁇ 4 hours
  • the detachable reaction sieve 11 is lifted from the fixed reaction vessel body 10 by the hooks 13-5 on the circulating chain conveyor 13, and the sieve of the detachable reaction sieve depends on gravity during the transportation process.
  • the barrier function of the net realizes the separation of the fiber and the pre-decomposition liquid.
  • the fiber pre-disintegration reactor 9 also includes a liftable stirring device 12 and a reactor cover, and the liftable stirring device includes a stirring paddle 12-3, a stirring motor 12-4,
  • the vertical fixing rod 12-2 and the lifting adjusting device 12-1, the lifting adjusting device 12-1 is sleeved on the vertical fixing rod, and can move up and down relative to the vertical fixing rod 12-2, the lifting adjusting device passes through the horizontal support rod 12 -5 is connected to the stirring motor 12-4, the stirring motor 12-4 is connected to the stirring paddle 12-3 in transmission, and the stirring paddle 12-3 is arranged vertically.
  • the reactor cover is opened, the fiber pre-decomposition liquid is added to the fixed reactor body 10, and the fibers are fed into the separable reaction sieve 11 and then immersed in the fiber pre-decomposition liquid. Then, the stirring paddle 12-3 is lowered to a suitable height through the lifting and adjusting device 12-1, and the fiber is pre-decomposed after closing the cover of the reactor.
  • the fiber pre-disintegration reactor 9 is also equipped with a heating device.
  • the separable reaction sieve 11 has a cylindrical frame structure, and the sieve body of the separable reaction sieve 11 is surrounded by a cylindrical sieve surface 11-1 to form a separable reaction
  • the bottom of the screen is a movable screen 1 1-3.
  • the left side of the movable screen 11-3 is hinged with the bottom of the reaction screen surface through a hinge 11-2.
  • the opening and closing of the movable screen is controlled by a mechanical switch.
  • the top of the separated reaction screen is also provided with a hoisting ring that is convenient for hoisting.
  • the above-mentioned separable reaction sieve 11 can also be arranged in a square frame structure or the like.
  • the mechanical switch can be designed as a spring link switch 11-6, the spring link switch 11-6 includes a first link 11-61 and a second link 11-62, and the first link 11-61 and The second connecting rods 11-62 are all arranged vertically, the first connecting rods 1 1-61 are connected to the screen body, the bottom of the first connecting rod is connected to the top of the second connecting rod through a spring 11-5, and the second connecting rod A horizontal bending part 11-4 for supporting the right side of the movable screen is formed at the bottom.
  • the opening and closing of the movable screen 11-3 is controlled by rotating the second connecting rod 11-62.
  • the horizontal bent portion 11-4 at the bottom end of the second connecting rod is rotated to the lower right side of the movable screen to support the movable screen and the fibrous materials on it.
  • the second connecting rod 11-62 is rotated so that the horizontal bending part 11-4 is no longer under the movable screen 11-3, that is, it is no longer given The supporting force of the movable screen.
  • the movable screen rotates along the hinge 11-2 under the action of gravity, and the fiber material on it is poured out under the action of gravity.
  • the spring 11_5 provides restoring force.
  • the mesh size of the above-mentioned reaction sieve surface 11-1 is 20 to 200 meshes, so as to adapt to materials of different fineness.
  • the circulating chain conveying device 13 includes a traction chain 13-2, a conveying track 13-1 and a hanging platform 13-3, and the traction chain 13-2 is drivingly connected with the conveying motor 13-4.
  • the hanging platform 13-3 is connected with the traction chain 13-2, and the hanging platform 13-3 is mounted on the conveying track 13-1.
  • the hanging platform 13-3 is driven by the conveying motor 13-4 through the traction chain 13-2 to run along the conveying track 13-1.
  • the bottom of the hanging platform 13-3 is provided with a hook 13-5, and the hook 13-5 is in phase with the lifting ring. Cooperate.
  • the conveying track 13-1 is undulating, that is, protrusions are provided at intervals in the extending direction of the conveying track.
  • the detachable reaction screen 11 is gradually moved under the traction of the traction chain, and constantly vibrates along with the undulating conveying track, and realizes the rapid separation of the fiber and the pre-decomposition liquid under the dual effects of vibration and gravity.
  • the circulating chain conveying device 13 has an oval shape, and the plane on which the circulating chain conveying device 13 is located It is inclined at an angle of 5° to 15° with respect to the horizontal plane, and gradually rises from the end close to the fiber pre-disintegration reactor 9 to the end of the second fiber temporary storage tank 15.
  • the circulating chain conveying device 13 is used to transfer the materials in the separable reaction screen 11 to the second fiber temporary storage tank 15, and the separable reaction screen 11 is returned to the fiber pre-disintegration reactor 9 for standby after the discharging of the separable reaction screen 11 is completed.
  • a pre-decomposition liquid recovery tank 14 is provided below the circulating chain conveying device 13, and the recovered pre-decomposition liquid is returned to the upper-level operation for recycling.
  • the fiber pre-decomposition liquid is added to the fixed reaction vessel body 10, and the fibers are fed into the separable reaction sieve 11 and then immersed in the fiber pre-decomposition liquid. Then, the liftable stirring device 12 is lowered to a suitable height, and the fiber is pre-decomposed after the cover of the reactor is closed.
  • the detachable reaction sieve 11 is lifted from the fixed reaction kettle body 10 by the hook on the circulating chain conveying device 13, and relies on the dual action of vibration and gravity during the conveying process to realize the separation of the fibers and the pre-decomposition liquid. Quick separation.
  • dl pre-decomposed fiber is fed into the second fiber temporary storage tank 15, and then fed into the material conveying belt 17 under the action of the third electric vibrating feeder 16.
  • the material conveying belt is arranged horizontally, and the upper part of the material conveying belt
  • Two water washing devices 18 and two functional modifier spraying devices 19 are respectively arranged in the material conveying direction, which are used to wash the materials and realize that the modifier fully wets the fibers.
  • the flushing water recovery tank 21 and the functional modifier recovery tank 22 are provided below the material conveying belt to realize the recovery and utilization of the flushing water and the functional modifier.
  • the photocatalytic microwave synergistic reactor 20 includes a shell, a fixed wavelength light source 20-1 is arranged on the top of the shell, and a microwave generator 20-2 is arranged on the left and right sides of the shell. .
  • the material conveying belt 17 passes through the bottom of the housing. The material to be processed is conveyed to the photocatalytic microwave synergistic reaction through the material conveying belt 17 In the reactor 20, under the combined action of the light emitted by the fixed wavelength light source 20-1 and the microwave generated by the microwave generator 20-2, the functional modification of the fiber is realized.
  • the above-mentioned fiber functional modification includes not only the oxidation of the active hydroxyl groups in the fiber structure (aldehyde grouping, ketonation and carboxylation), but also the amination, sulfonation and nitration of active reactive sites, etc. , It also includes the grafting reaction of the fiber structure.
  • the fineness of the functionalized fiber prepared by the present invention is 1-2 mm, and has good dispersibility.
  • the pre-decomposition liquid is composed of 3.0 parts by mass 30% hydrogen peroxide, 1.0 parts potassium persulfate, 0.5 parts cobalt chloride accelerator and 95.5 parts water, using 1mol/L Adjust the pH of the pre-decomposition liquid to 8 with the sodium hydroxide solution.
  • the fiber is dehydrated, washed, and then sprayed with a functional modifier, and then transported to the photocatalytic microwave synergistic reactor 20 for functional modification to prepare a functional fiber.
  • the reaction light source uses a 254nm ultraviolet lamp, and the microwave reactor power is set to 600W.
  • the functional modifier is hydrolyzed by 20 parts by mass of graphene oxide solution with a concentration of 0.5% and 60 parts by mass of a KH-550/A-151 composite silane coupling agent with a concentration of 2%. Liquid (the mass ratio of silane coupling agent KH-550 to A-151 is 1:1) and 20 parts of ionic liquid.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Fertilizers (AREA)
  • Processing Of Solid Wastes (AREA)
  • Treatment Of Sludge (AREA)

Abstract

L'invention concerne un procédé de préparation de fibre fonctionnalisée superfine à l'aide de drêches de distillerie, comprenant les étapes suivantes : a) la pulvérisation par cisaillement à grande vitesse de drêches de distillerie ; b) la séparation et l'extraction de la fibre de drêches de distillerie ; c) la pré-décomposition de la fibre de drêches de distillerie ; et d) la modification de fonctionnalisation de fibre. Dans le procédé, la modification de fibre est divisée en deux procédures, à savoir une pré-décomposition et une modification de fonctionnalisation. Sous l'action d'un liquide de pré-décomposition fabriqué, la rupture des liaisons oxygène en pont dans la fibre est rapidement obtenue, augmentant fortement le nombre de sites actifs pour une modification ultérieure ainsi que l'efficacité et le degré de modification de fibre; ensuite, la pulvérisation d'un agent de modification de fonctionnalisation est effectuée; puis une modification de fonctionnalisation de fibre est mise en œuvre sous l'action combinée d'une source de lumière à longueur d'onde fixe et de micro-ondes afin d'obtenir la fibre fonctionnalisée superfine. Dans le procédé, différents types d'agents de modification peuvent être utilisés pour effectuer une modification de fonctionnalisation sur la fibre, de telle sorte que la fibre fonctionnalisée superfine modifiée peut être utilisée dans les domaines de la modification de bouillie de ciment et de la modification de produits de revêtement. Ainsi, l'invention permet d'obtenir un procédé viable pour l'utilisation efficace de drêches de distillerie, et la valeur économique et d'utilisation de produits associés aux drêches de distillerie peut être considérablement augmentée.
PCT/CN2020/082853 2020-02-25 2020-04-01 Procédé de préparation de fibre fonctionnalisée superfine à l'aide de drêches de distillerie Ceased WO2021051780A1 (fr)

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