CN113981726A - Method for producing needle-leaved refined cellulose by biological defibering - Google Patents
Method for producing needle-leaved refined cellulose by biological defibering Download PDFInfo
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- CN113981726A CN113981726A CN202111275762.9A CN202111275762A CN113981726A CN 113981726 A CN113981726 A CN 113981726A CN 202111275762 A CN202111275762 A CN 202111275762A CN 113981726 A CN113981726 A CN 113981726A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
- C12N11/14—Enzymes or microbial cells immobilised on or in an inorganic carrier
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
- C12N9/0004—Oxidoreductases (1.)
- C12N9/0055—Oxidoreductases (1.) acting on diphenols and related substances as donors (1.10)
- C12N9/0057—Oxidoreductases (1.) acting on diphenols and related substances as donors (1.10) with oxygen as acceptor (1.10.3)
- C12N9/0061—Laccase (1.10.3.2)
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12Y—ENZYMES
- C12Y110/00—Oxidoreductases acting on diphenols and related substances as donors (1.10)
- C12Y110/03—Oxidoreductases acting on diphenols and related substances as donors (1.10) with an oxygen as acceptor (1.10.3)
- C12Y110/03002—Laccase (1.10.3.2)
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/02—Pretreatment of the raw materials by chemical or physical means
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
- D21B1/00—Fibrous raw materials or their mechanical treatment
- D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
- D21B1/06—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by dry methods
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/20—Methods of refining
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- Chemical Or Physical Treatment Of Fibers (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
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Abstract
The invention discloses a method for defibering and producing needle-leaved refined cellulose by a biological method, which comprises the following steps: p1, obtaining a crushed raw material; p2, obtaining a soaking raw material; p3, obtaining a heat preservation raw material; p4, obtaining a carrier with enzyme; p5, obtaining a reaction raw material; p6, obtaining a filter raw material; p7, putting the filtered raw material into a pulping machine for pulping and defibering to obtain defibered raw material; p8, will discongest in the raw materials drops into the drying-machine, dry, can accomplish the preparation of refined cellulose, through carrying out the breakage to the needle leaf raw materials and soaking, increase its flexibility, the micropore ball carrier that combines argil preparation comes the attached laccase as biological treatment agent, guarantee the efficiency and the stability of enzymolysis, avoid losing, can effectively improve the dispersed fineness of cellulose, avoid the caking, can improve the efficiency and the quality of refined cellulose preparation greatly like this, guarantee the process safety, facilitate the use widely.
Description
Technical Field
The invention relates to the technical field of needle leaf cellulose, in particular to a method for defibering and producing needle leaf refined cellulose by using a biological method.
Background
When the needle leaves are used for preparing refined cellulose, needle leaf raw materials need to be processed through a cutting procedure, and finally cellulose products are formed and further applied to different fields.
However, in the existing preparation of needle-leaf refined cellulose, mechanical treatment is mostly adopted, so that the energy consumption is large, the pollution is serious, the defibering and dispersing effects on cellulose are poor, more fiber bundles are easily mixed, the quality of cellulose is reduced, and in some processes of preparation by an enzymolysis mode, enzyme is mostly directly put into cellulose pulp, so that the attachment stability of the enzyme cannot be ensured, the comprehensive contact with the cellulose cannot be ensured, the enzymolysis efficiency and quality are influenced, and finally, the stable separation is not facilitated, and a new method needs to be provided.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for defibering and producing needle-leaved refined cellulose by using a biological method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for defibering and producing needle leaf refined cellulose by a biological method comprises the following steps:
p1, selecting needle leaf raw materials, cleaning, dedusting and crushing to obtain crushed raw materials;
p2, putting the crushed raw materials into a soaking pool, adding clear water according to the weight ratio of 1:5-8, heating to 80-90 ℃, soaking and cooking the crushed raw materials for 2-3 hours, and naturally cooling to obtain soaked raw materials;
p3, adding the soaking raw material and soaking water into a reaction tank together, heating to 30-35 ℃, and preserving heat to obtain a heat preservation raw material;
p4, preparing a microporous ball carrier, putting the microporous ball carrier into an enzyme culture medium, and performing amplification culture to obtain an enzyme carrier;
p5, uniformly putting the carrier with the enzyme into the heat-preservation raw material, heating to 55-60 ℃, preserving heat, standing for 24-32 hours, and reacting to obtain a reaction raw material;
p6, taking out the reaction raw material, filtering, removing the carrier with the enzyme and redundant water, and ensuring that the water content of the raw material is 30-40% to obtain a filtered raw material;
p7, putting the filtered raw material into a pulping machine for pulping and defibering to obtain defibered raw material;
and P8, putting the defibering raw materials into a dryer, and drying to finish the preparation of the refined cellulose.
Preferably, the dried needle leaf raw material is selected from the P1, crushed to 20-50 meshes, and filtered and sieved by a screen.
Preferably, the P2 further comprises stirring the crushed raw materials at a stirring speed of 80-120 rpm for 15-18 minutes.
Preferably, the method for preparing the microporous sphere carrier in P4 comprises the following steps:
a1, selecting argil as a carrier raw material, and crushing and grinding the argil to form argil powder;
a2, adding water into the argil powder, and uniformly stirring to prepare a mud plate structure;
a3, cutting the mud plate structure to form mud blocks;
a4, wrapping steel balls in the mud blocks, then putting the mud blocks into sawdust to roll, and forming wrapped mud balls when the surface is not full of sawdust;
a5, placing the wrapped mud balls in a cool environment, drying in the shade, and placing for 8 to 12 hours to obtain dried mud balls in the shade;
a6, putting the dried mud balls into a sintering furnace, sintering and molding at 500-650 ℃, burning and carbonizing the powder, and forming a microporous structure on the surface to obtain a microporous ball blank;
and A7, soaking and washing the microporous ball blank in water, and then drying to finish the preparation of the microporous ball carrier.
Preferably, the method for obtaining the carrier with the enzyme by expanding culture in the P4 comprises the following steps:
b1, putting laccase as a defibering organism into a liquid culture medium, and culturing for 3 to 5 days;
b2, adding catalase and hydrogen peroxide solution with the mass fraction of 30% into the liquid culture medium, uniformly stirring for 5 to 8 minutes, and standing and culturing for 30 to 40 minutes;
b3, concentrating the liquid culture medium until the water content is 50% -55% to form a concentrated culture solution;
and B4, putting the microporous spherical carrier into a concentrated culture medium, shaking and stirring, and immersing the laccase into pores on the surface of the microporous spherical carrier to obtain the carrier with the enzyme.
Preferably, the method for removing the carrier with the enzyme in the P6 comprises the following steps:
c1, electrifying an electromagnet to insert the electromagnet into the reaction raw material, and taking the magnetic adsorption steel beads out of the enzyme carrier;
c2, putting the carrier with the enzyme into a gauze, washing the carrier with clear water to form washing liquid, C3, adding the washing liquid into the reaction solution, heating and concentrating the solution at 70-80 ℃, connecting a steam pipeline with a condenser to condense and recover the solution to obtain concentrated reaction solution;
and C4, filtering the concentrated reaction solution to remove surface floating substances and foams to obtain a filtering raw material.
Preferably, the refining speed in the P7 is 120-130 revolutions per minute, the solid-liquid ratio is 1:3-4, and the refining time is 30-45 minutes.
Preferably, the untwining speed in the P7 is 3000 rpm to 3500 rpm, and the fiber grading treatment is carried out by a standard Baol sieve separator.
Preferably, the dryer in the step P8 is a hot air dryer, the drying temperature is 55 to 60 ℃, the air volume is 30 to 45 liters per minute, and the water content is 5 to 8 percent during drying.
According to the method for defibering and producing needle-leaved refined cellulose by using the biological method, needle-leaved raw materials are crushed and soaked, the flexibility of the needle-leaved raw materials is increased, laccase is attached to a microporous ball carrier made of pottery clay to serve as a biological treatment agent, the needle-leaved raw materials can be stably and comprehensively contacted with cellulose after being attached, the enzymolysis efficiency and stability are guaranteed, loss is avoided, magnetic adsorption can be used for separation, residues are avoided, the filtering efficiency and safety are guaranteed, pulping and defibering are carried out after enzymolysis, the fineness of cellulose dispersion can be effectively improved, agglomeration is avoided, the preparation efficiency and quality of the refined cellulose can be greatly improved, the process safety is guaranteed, and the method is convenient to popularize and use.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A method for defibering and producing needle leaf refined cellulose by a biological method comprises the following steps:
p1, selecting needle leaf raw materials, cleaning, dedusting and crushing to obtain crushed raw materials;
p2, putting the crushed raw materials into a soaking pool, adding clear water according to the weight ratio of 1:5-8, heating to 80-90 ℃, soaking and cooking the crushed raw materials for 2-3 hours, and naturally cooling to obtain soaked raw materials;
p3, adding the soaking raw material and soaking water into a reaction tank together, heating to 30-35 ℃, and preserving heat to obtain a heat preservation raw material;
p4, preparing a microporous ball carrier, putting the microporous ball carrier into an enzyme culture medium, and performing amplification culture to obtain an enzyme carrier;
p5, uniformly putting the carrier with the enzyme into the heat-preservation raw material, heating to 55-60 ℃, preserving heat, standing for 24-32 hours, and reacting to obtain a reaction raw material;
p6, taking out the reaction raw material, filtering, removing the carrier with the enzyme and redundant water, and ensuring that the water content of the raw material is 30-40% to obtain a filtered raw material;
p7, putting the filtered raw material into a pulping machine for pulping and defibering to obtain defibered raw material;
and P8, putting the defibering raw materials into a dryer, and drying to finish the preparation of the refined cellulose.
Preferably, the dried needle leaf raw material is selected from the P1, crushed to 20-50 meshes, and filtered and sieved by a screen.
Preferably, the P2 further comprises stirring the crushed raw materials at a stirring speed of 80-120 rpm for 15-18 minutes.
Preferably, the method for preparing the microporous sphere carrier in P4 comprises the following steps:
a1, selecting argil as a carrier raw material, and crushing and grinding the argil to form argil powder;
a2, adding water into the argil powder, and uniformly stirring to prepare a mud plate structure;
a3, cutting the mud plate structure to form mud blocks;
a4, wrapping steel balls in the mud blocks, then putting the mud blocks into sawdust to roll, and forming wrapped mud balls when the surface is not full of sawdust;
a5, placing the wrapped mud balls in a cool environment, drying in the shade, and placing for 8 to 12 hours to obtain dried mud balls in the shade;
a6, putting the dried mud balls into a sintering furnace, sintering and molding at 500-650 ℃, burning and carbonizing the powder, and forming a microporous structure on the surface to obtain a microporous ball blank;
and A7, soaking and washing the microporous ball blank in water, and then drying to finish the preparation of the microporous ball carrier.
Preferably, the method for obtaining the carrier with the enzyme by expanding culture in the P4 comprises the following steps:
b1, putting laccase as a defibering organism into a liquid culture medium, and culturing for 3 to 5 days;
b2, adding catalase and hydrogen peroxide solution with the mass fraction of 30% into the liquid culture medium, uniformly stirring for 5 to 8 minutes, and standing and culturing for 30 to 40 minutes;
b3, concentrating the liquid culture medium until the water content is 50% -55% to form a concentrated culture solution;
and B4, putting the microporous spherical carrier into a concentrated culture medium, shaking and stirring, and immersing the laccase into pores on the surface of the microporous spherical carrier to obtain the carrier with the enzyme.
Preferably, the method for removing the carrier with the enzyme in the P6 comprises the following steps:
c1, electrifying an electromagnet to insert the electromagnet into the reaction raw material, and taking the magnetic adsorption steel beads out of the enzyme carrier;
c2, putting the carrier with the enzyme into a gauze, washing the carrier with clear water to form washing liquid, C3, adding the washing liquid into the reaction solution, heating and concentrating the solution at 70-80 ℃, connecting a steam pipeline with a condenser to condense and recover the solution to obtain concentrated reaction solution;
and C4, filtering the concentrated reaction solution to remove surface floating substances and foams to obtain a filtering raw material.
Preferably, the refining speed in the P7 is 120-130 revolutions per minute, the solid-liquid ratio is 1:3-4, and the refining time is 30-45 minutes.
Preferably, the untwining speed in the P7 is 3000 rpm to 3500 rpm, and the fiber grading treatment is carried out by a standard Baol sieve.
Preferably, the dryer in the step P8 is a hot air dryer, the drying temperature is 55 to 60 ℃, the air volume is 30 to 45 liters per minute, and the water content is 5 to 8 percent during drying.
Claims (9)
1. A method for defibering and producing needle-leaved refined cellulose by a biological method is characterized by comprising the following steps: the method for defibering and producing the needle-leaved refined cellulose by using the biological method comprises the following steps:
p1, selecting needle leaf raw materials, cleaning, dedusting and crushing to obtain crushed raw materials;
p2, putting the crushed raw materials into a soaking pool, adding clear water according to the weight ratio of 1:5-8, heating to 80-90 ℃, soaking and cooking the crushed raw materials for 2-3 hours, and naturally cooling to obtain soaked raw materials;
p3, adding the soaking raw material and soaking water into a reaction tank together, heating to 30-35 ℃, and preserving heat to obtain a heat preservation raw material;
p4, preparing a microporous ball carrier, putting the microporous ball carrier into an enzyme culture medium, and performing amplification culture to obtain an enzyme carrier;
p5, uniformly putting the carrier with the enzyme into the heat-preservation raw material, heating to 55-60 ℃, preserving heat, standing for 24-32 hours, and reacting to obtain a reaction raw material;
p6, taking out the reaction raw material, filtering, removing the carrier with the enzyme and redundant water, and ensuring that the water content of the raw material is 30-40% to obtain a filtered raw material;
p7, putting the filtered raw material into a pulping machine for pulping and defibering to obtain defibered raw material;
and P8, putting the defibering raw materials into a dryer, and drying to finish the preparation of the refined cellulose.
2. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the dried needle leaf raw material is selected from the P1, crushed to 20-50 meshes and filtered and sieved by a screen mesh.
3. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the P2 also comprises stirring the crushed raw materials, wherein the stirring speed is 80-120 revolutions per minute for 15-18 minutes.
4. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the method for manufacturing the microporous sphere carrier in P4 comprises the following steps:
a1, selecting argil as a carrier raw material, and crushing and grinding the argil to form argil powder;
a2, adding water into the argil powder, and uniformly stirring to prepare a mud plate structure;
a3, cutting the mud plate structure to form mud blocks;
a4, wrapping steel balls in the mud blocks, then putting the mud blocks into sawdust to roll, and forming wrapped mud balls when the surface is not full of sawdust;
a5, placing the wrapped mud balls in a cool environment, drying in the shade, and placing for 8 to 12 hours to obtain dried mud balls in the shade;
a6, putting the dried mud balls into a sintering furnace, sintering and molding at 500-650 ℃, burning and carbonizing the powder, and forming a microporous structure on the surface to obtain a microporous ball blank;
and A7, soaking and washing the microporous ball blank in water, and then drying to finish the preparation of the microporous ball carrier.
5. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the method for obtaining the carrier with the enzyme by the amplification culture in the P4 comprises the following steps:
b1, putting laccase as a defibering organism into a liquid culture medium, and culturing for 3 to 5 days;
b2, adding catalase and hydrogen peroxide solution with the mass fraction of 30% into the liquid culture medium, uniformly stirring for 5 to 8 minutes, and standing and culturing for 30 to 40 minutes;
b3, concentrating the liquid culture medium until the water content is 50% -55% to form a concentrated culture solution;
and B4, putting the microporous spherical carrier into a concentrated culture medium, shaking and stirring, and immersing the laccase into pores on the surface of the microporous spherical carrier to obtain the carrier with the enzyme.
6. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the method for removing the carrier with the enzyme in the P6 comprises the following steps:
c1, electrifying an electromagnet to insert the electromagnet into the reaction raw material, and taking the magnetic adsorption steel beads out of the enzyme carrier;
c2, putting the carrier with enzyme into the gauze, washing with clean water to form a washing liquid,
C3, adding the flushing liquid into the reaction solution, heating and concentrating the solution when the temperature is between 70 and 80 ℃, and connecting a steam pipeline with a condenser for condensation and recovery to obtain a concentrated reaction solution;
and C4, filtering the concentrated reaction solution to remove surface floating substances and foams to obtain a filtering raw material.
7. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the refining speed in the P7 is 120-130 r/min, the solid-liquid ratio is 1:3-4, and the refining lasts for 30-45 minutes.
8. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the untwining speed in the P7 is 3000-3500 rpm, and fiber grading treatment is carried out by a standard Baol sieve separator.
9. The method for defibering and producing needle-leaved refined cellulose according to claim 1, wherein the steps of: the dryer in the step P8 is a hot air dryer, the drying temperature is 55-60 ℃, the air volume is 30-45 liters per minute, and the water content is 5-8% during drying.
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| CN202111275762.9A CN113981726A (en) | 2021-10-29 | 2021-10-29 | Method for producing needle-leaved refined cellulose by biological defibering |
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| CN202111275762.9A CN113981726A (en) | 2021-10-29 | 2021-10-29 | Method for producing needle-leaved refined cellulose by biological defibering |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212582A (en) * | 2011-04-12 | 2011-10-12 | 王美岭 | Method for preparing cellulose from straws by using biological method |
| CN107698773A (en) * | 2017-09-15 | 2018-02-16 | 江苏大学 | A kind of magnetic dendritic composite nanoparticle and its preparation method and application |
| CN111472190A (en) * | 2020-03-09 | 2020-07-31 | 齐齐哈尔大学 | Method for extracting high-purity straw cellulose by utilizing immobilized enzyme technology for pretreatment |
-
2021
- 2021-10-29 CN CN202111275762.9A patent/CN113981726A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212582A (en) * | 2011-04-12 | 2011-10-12 | 王美岭 | Method for preparing cellulose from straws by using biological method |
| CN107698773A (en) * | 2017-09-15 | 2018-02-16 | 江苏大学 | A kind of magnetic dendritic composite nanoparticle and its preparation method and application |
| CN111472190A (en) * | 2020-03-09 | 2020-07-31 | 齐齐哈尔大学 | Method for extracting high-purity straw cellulose by utilizing immobilized enzyme technology for pretreatment |
Non-Patent Citations (1)
| Title |
|---|
| 王苗苗等: "介孔SiO_2/Fe_3O_4中空磁性微球的漆酶固定化", 《高等学校化学学报》 * |
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Application publication date: 20220128 |