CN113417164A - Production method of powdery cellulose - Google Patents
Production method of powdery cellulose Download PDFInfo
- Publication number
- CN113417164A CN113417164A CN202110847794.5A CN202110847794A CN113417164A CN 113417164 A CN113417164 A CN 113417164A CN 202110847794 A CN202110847794 A CN 202110847794A CN 113417164 A CN113417164 A CN 113417164A
- Authority
- CN
- China
- Prior art keywords
- cellulose
- crushing
- powdery cellulose
- feeding
- hydrochloric acid
- 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.)
- Pending
Links
Images
Classifications
-
- 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
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention belongs to the field of preparation of high molecular compounds, and relates to a method for producing powdery cellulose, which comprises the following steps: s1, adding a low-concentration hydrochloric acid solution into wood pulp, and preserving heat for 1.5 to 2 hours at the temperature of 60 to 80 ℃ to obtain a slurry material; the mass concentration of the hydrochloric acid solution is 0.03-0.05%; s2, performing filter pressing on the slurry material, and collecting a filter cake; s3, drying the filter cake; and S4, crushing the dried filter cake to obtain powdery cellulose. The invention adopts a production process of preparing powdery cellulose by partially depolymerizing cellulose under the action of chemical energy and then crushing the cellulose by using mechanical energy. Hydrolysis of the fibers by very low concentrations of inorganic acids controls the degree of polymerization and partially depolymerizes the cellulose polymer. After the cellulose is partially degraded by the action of chemical energy, the molecular chain length is shortened under the action of the chemical energy, the strength of the cellulose is reduced, and the cellulose is more easily crushed by mechanical energy to obtain powdery cellulose with different levels of physical property indexes.
Description
Technical Field
The invention belongs to the field of preparation of high molecular compounds, relates to a preparation method of cellulose, and particularly relates to a production method of powdery cellulose.
Background
Cellulose is the oldest and most abundant natural polymer on the earth, is inexhaustible, and is the most precious natural renewable resource for human beings. Cellulose is a polysaccharide which is widely distributed and has the largest content in the nature, and accounts for more than 50 percent of the carbon content in the plant. The cellulose content of cotton is close to 100%, and is the purest cellulose source in nature. In general wood, cellulose accounts for 40-50%, hemicellulose accounts for 10-30%, and lignin accounts for 20-30%. Cellulose is a substance which is not digested and absorbed by human beings, but has important effects on the aspects of ensuring human health and prolonging life, and is called as a seventh nutrient.
Cellulose is a bulk substance, has poor fluidity and little surface hydroxyl exposure, is not beneficial to the application of the cellulose, and the cellulose needs to be prepared into a powdery form from the bulk so as to endow the cellulose with new functions. The powdered cellulose products with different forms and different types are produced through technical research, and the cellulose products are in the forms of fine powder or solid particles with good fluidity to coarse, fluffy and non-flowable in different fineness, bulk specific gravity, fiber length, granularity and particle size, so that the use requirements of different application fields on the cellulose are met.
The powdery cellulose microstructure is ribbon-shaped and bent, rugged, porous, flat at the intersection, good in toughness, dispersibility, chemical stability and water absorption capacity, so that the powdery cellulose microstructure has wide application in the fields of pharmacy, food, cosmetics and industry, and can be applied to the aspects of building, electric power, oil processing, metallurgy, chemical fiber, printing and dyeing, filtering materials, friction materials, sealing gaskets, environmental protection, sewage treatment, seawater desalination, sulfonate refining and the like. The coating is widely applied to the fields of concrete, mortar, gypsum products, wood pulp sponge, asphalt roads and the like, and has good effects of preventing coating cracking, improving water retention, improving production stability and construction convenience, increasing strength, enhancing adhesion to the surface and the like.
The powdery cellulose developed at home in the current market is not similar to foreign products in the main indexes of the product such as color, average fiber length, water soluble substance content, heavy metal content and the like. The medical grade, food grade and even industrial grade high-end powdery cellulose has high quality requirement, the powdery cellulose used in China is imported from Germany, America, Japan and other countries, and foreign known enterprises such as Solvira Specialties Inc., Germany Jeluwerk FMK company and Germany JRS Rudenmeil cellulose company have good quality but high price. The powdery cellulose production enterprises with the scale above China are almost not available.
The deep processing of the bulk cellulose in China starts late, only simple crushing is needed, the bulk specific gravity of the product is light, the particle size is coarse, the fluidity is poor, and the application range is limited. At present, the main production process for domestic and foreign research and production of powdered cellulose is to use mechanical pulverization, i.e. mechanical pulverization is used to reduce the particle size of cellulose and convert purified cellulose pulp into powdered cellulose. The process has obvious defects: because the connection strength between the fibers is high, multiple times of crushing and multiple times of grinding are needed in the preparation process, the mechanical energy consumption is high, the cost is high, and the particle size of the produced powdery cellulose is relatively large. Therefore, how to simply and efficiently solve the technical difficulties, develop and research a new process method for producing powdery cellulose, form industrialized production and have important social and economic significance.
Disclosure of Invention
The invention aims to overcome the defects of the preparation of the powdery cellulose in the prior art, and provides a production method of the powdery cellulose, so that the powdery cellulose with various indexes meeting the standard of the powdery cellulose and better flowability is obtained.
The invention adopts the following technical scheme:
a method for producing powdery cellulose comprises the following steps:
s1, adding a low-concentration hydrochloric acid solution into wood pulp, and preserving heat for 1.5 to 2 hours at the temperature of 60 to 80 ℃ to obtain a slurry material; the mass concentration of the hydrochloric acid solution is 0.03-0.05%;
s2, performing filter pressing on the slurry material, and collecting a filter cake;
s3, drying the filter cake;
and S4, crushing the dried filter cake to obtain powdery cellulose.
The technical scheme adopts a production process of preparing the powdery cellulose by partially depolymerizing the cellulose through the action of chemical energy and then crushing the cellulose by using mechanical energy. Hydrolysis of the fibers by very low concentrations of inorganic acids controls the degree of polymerization and partially depolymerizes the cellulose polymer. After the cellulose is partially degraded by the action of chemical energy, the molecular chain length is shortened under the action of the chemical energy, the strength of the cellulose is reduced, the cellulose is more easily crushed by mechanical energy, and powdery cellulose with different grades of physical property indexes can be prepared. The cellulose partially degraded by the chemical energy is reduced in fiber strength due to the reduction of the length of a molecular chain, and then is mechanically crushed, so that the cellulose is more easily crushed into powdery cellulose with finer granularity and better fluidity by mechanical energy.
In the prior art, only acid hydrolysis is adopted for preparing microcrystalline cellulose, and according to the conventional understanding in the field, powdery cellulose cannot be obtained by acid hydrolysis, but microcrystalline cellulose with lower polymerization degree is obtained.
The invention breaks through the inertial thinking, controls the polymerization degree of cellulose by adjusting the acidolysis process conditions and adopting hydrochloric acid solution with extremely low concentration, and the cellulose is powdery cellulose with the polymerization degree of more than or equal to 500 generally. If the acid concentration is too high, the temperature is too high, the hydrolysis speed is too high, the reaction process is difficult to control, excessive acidolysis is caused, and the microcrystalline cellulose possibly degraded into the microcrystalline cellulose can lose the characteristics of the powdery cellulose of the target product; if the acid concentration is too low, the temperature is too low, and the reaction speed is too slow, the toughness of the cellulose cannot be reduced, and the subsequent mechanical crushing processing is influenced. The process research controls the concentration of hydrochloric acid at 0.03-0.05%, and controls the acidolysis reaction temperature at 60-80 ℃ to carry out acidolysis test, thus obtaining the best acidolysis effect.
In addition, even if the acidolysis time is too long within the hydrochloric acid concentration, the cellulose can not be subjected to excessive acidolysis to form microcrystalline cellulose, and the applicant has made relevant experiments, and the cellulose is subjected to acidolysis for 2h, 4h, 6h, 8h and 10h at the hydrochloric acid concentration of 0.03% and the temperature of 75 ℃, and the corresponding polymerization degrees are 591, 573, 562, 550 and 541, so that the polymerization degree requirement of the powdery cellulose is still met.
Preferably, the solids content of the wood pulp is controlled to be 20 to 25% after addition of the hydrochloric acid solution.
Preferably, the filter cake in the step (S2) is washed to neutrality with clean water.
Preferably, after the step (S1), the treatment is repeated once with the hydrochloric acid solution of the same concentration at a temperature of 20 to 40 ℃. The first acidolysis is carried out at a higher temperature, which is beneficial to the depolymerization of cellulose, and then the acidolysis is repeated at a lower temperature, at the moment, the molecular motion in the solution is slowed down, the cellulose with longer molecular chains which do not reach the polymerization degree requirement of the powdery cellulose is continuously depolymerized, and the cellulose which reaches the polymerization degree requirement is not continuously depolymerized into microcrystalline cellulose. Ensuring that the degree of polymerisation of the powdered cellulose is still maintained under the acid treatment conditions.
Preferably, after the acid hydrolysis and before the press filtration (i.e., between step S1 and step S2), the slurry material is subjected to a beating process, so that it is more easily pulverized and refined, and pulverized and ground into a powdery cellulose product having a finer particle size, a higher bulk specific gravity, and a better fluidity. The principle of the method is that after the cellulose is partially degraded by the action of chemical energy, the molecular chain length is shortened under the action of the chemical energy, the strength of the cellulose is reduced, the cellulose is more easily crushed, refined, crushed and ground by mechanical energy, and powdery cellulose with different grades of physical property indexes can be prepared.
Preferably, in the step (S4), the pulverization is carried out by a pulverizer dedicated to the pulverization of cellulose, and the pulverization is carried out by a combination of plural forms of grinding, shearing and collision.
This rubbing crusher includes: the device comprises a feeding part, a crushing part communicated with the feeding part and a grading part communicated with the crushing part, wherein the feeding part is provided with a feeding hole, and the grading part is provided with a discharging hole.
Preferably, the feeding part comprises a feeding bin, an outlet of the feeding bin is communicated with the crushing part, and a feeding rotating wheel which is driven by a motor to rotate and is transversely arranged is arranged in the feeding bin.
Preferably, the edges of the runner blades of the feed runner are provided with serrations.
Preferably, the outer end of the runner blade of the feeding runner is in a conical structure.
Preferably, the crushing component comprises a crushing box and a crushing structure arranged in the crushing box, the crushing structure comprises a main shaft, an auxiliary shaft arranged around the main shaft and a grinding wheel arranged on the auxiliary shaft, the main shaft is driven by a motor to rotate, and the auxiliary shaft is driven by the main shaft to rotate.
Preferably, a gap between the grinding wheel and an inner wall of the crushing box is not more than 1.5 cm. Therefore, a grinding area is formed between the grinding wheel and the inner wall of the crushing box, and materials in the grinding area are fully ground in the continuous rotating process of the grinding wheel.
Preferably, the grinding wheels are rotatably connected to the auxiliary shafts, and when the main shaft rotates, the grinding wheels not only revolve around the main shaft, but also rotate around the respective auxiliary shafts, so that the grinding, shearing and colliding actions are simultaneously realized, and the cellulose crushing effect is improved.
Preferably, the outer surface of the grinding wheel is provided with blades, and the blades are spirally arranged along the axial direction of the grinding wheel.
Preferably, a rotor frame is provided at an upper end of the main shaft, and the sub-shaft is mounted to the rotor frame.
Preferably, the lower surface of rotor frame is provided with scraper structure, scraper structure including set up in scraper axle on the rotor frame with set up in the scraper of scraper axle front end, the scraper is located the emery wheel below.
Preferably, the classification part comprises a classification box arranged above the crushing box and a classification disc arranged in the classification box, a discharge port connected with a suction device is arranged above the classification disc, and an air inlet is further formed in the crushing box.
Preferably, the product fineness is adjusted according to the rotating speed of the grading disc along the discharge hole direction of the powdered cellulose, so that different types of powdered cellulose can be produced.
The grinding wheel continuously and integrally moves with the grinder to grind, shear and collide by the centrifugal force of the grinding wheel, so that the cellulose is crushed and sheared horizontally and vertically to improve the grinding efficiency, the fineness of the powdery cellulose is finer, the bulk density is higher, the flowability of powder is better, and products with different models and capable of meeting market demands can be produced by adjusting process parameters.
Through the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the production process of preparing the powdery cellulose by partially depolymerizing cellulose under the action of chemical energy and then crushing the cellulose by using mechanical energy is adopted. Hydrolysis of the fibers by very low concentrations of inorganic acids controls the degree of polymerization and partially depolymerizes the cellulose polymer. After the cellulose is partially degraded by the action of chemical energy, the molecular chain length is shortened under the action of the chemical energy, the strength of the cellulose is reduced, and the cellulose is more easily crushed by mechanical energy to obtain powdery cellulose with different levels of physical property indexes.
2. Compared with the pure mechanical pulverization in the prior art, the preparation cost is lower.
3. The pulverizer provided by the invention continuously and integrally moves with the pulverizer for grinding, shearing and colliding by the centrifugal force of the grinding wheel, so that cellulose is crushed and sheared in the horizontal direction and the vertical direction to improve the crushing efficiency, the fineness of the powdery cellulose is finer, the bulk density is higher, the flowability of powder is better, and products with different models and capable of meeting market requirements can be produced by adjusting process parameters.
Drawings
FIG. 1 is a schematic view of a pulverizer according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a feeding unit of a pulverizer according to an embodiment of the present invention;
FIG. 3 is a schematic view of the feed rotor of the pulverizer shown in one embodiment of the present invention;
FIG. 4 is a schematic structural view of a rotor blade of a pulverizer according to an embodiment of the present invention
FIG. 5 is a schematic view of the crushing member of the crusher according to one embodiment of the present invention;
FIG. 6 is a schematic view showing the structure of a classifying plate of a pulverizer according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a method for producing powdery cellulose comprises the following steps:
raw materials: food-grade wood pulp: content of α -cellulose: 96.8 percent; ash content: 0.06 percent; loss on drying: 7.8 percent; polymerization degree: 1073.
hydrochloric acid: total acidity: 31 percent; reduction product: < 0.007%.
1. 1500kg of deionized water was added to a 2000L enamel reactor, the stirrer was started, and 1.5kg of concentrated hydrochloric acid (about 31% by mass) was slowly added to prepare a 0.03% diluted hydrochloric acid solution. 500kg of food-grade wood pulp is slowly added into a 4000L novel double-shaft differential high-shear reaction device, a spacer steam heating switch is started, and simultaneously, a prepared dilute hydrochloric acid solution is injected. Wood pulp is swelled, mixed and sheared and depolymerized in a novel double-shaft differential high-shear horizontal reaction kettle to prepare a wood pulp mixture with the solid content of 24.8%, and the wood pulp mixture is heated to 75 ℃ and is kept for continuous depolymerization for 2 hours.
2. Keeping the temperature for continuous depolymerization to obtain a crude cellulose product, observing an aqueous dispersion solution with the solid content of 1% by using a microscope, depolymerizing the cellulose from a bulk state to a long fiber state, obviously shortening the fiber length, and detecting the polymerization degree to be 589.
3. Stopping heating after depolymerization is finished, stirring to obtain a slurry material, adding water to dilute the slurry material until the content is about 10%, pulping for 1 hour by using a vertical three-stage high-speed high-shear cellulose refining dispersion machine, pumping the obtained slurry into a plate-and-frame filter press for filter pressing, rinsing with deionized water to be neutral to obtain a cellulose crude product with the solid content of 45.8%, and the wet filter cake content of 986.2kg, wherein the yield is 97.98% (calculated on dry products). The cellulose is dried by a high shear granulation dryer.
4. Drying at the air inlet temperature of 150 ℃ and 200 ℃ and the air outlet temperature of 70-80 ℃ in the high-shear granulation drying device.
5. Crushing: the depolymerized cellulose is crushed into powder by a special crusher for cellulose micronization in a mode of combining various forms of grinding, shearing and collision, and the powder cellulose product passes through a 60-mesh screen, so that the drying weight loss of the powder cellulose product is 3.9 percent, the weight is 449.8kg, the yield is 95.7 percent (calculated by dry product), and the bulk specific gravity is 0.26g/cm3The angle of repose was 47.1 °.
Comparative materials: food additive powdered cellulose Justfiber BH200
JustFiber BH200 is a purified powdered cellulose obtained by treating alpha-cellulose, obtainable from cellulose-containing plant fiber pulp, having a high bulk density and good flowability. Manufactured by international cellulose corporation (IFC) Solvaira Specialties Inc of north tonneaux, new york, usa. It is used in the food industry as dietary fiber, has anti-adhesion or carrier material function, and has high chemical and microbial purity. Is an odorless and tasteless ingredient effective for reducing the caloric content of a food product, and is free of calories, fats, and digestible carbohydrates. Can be used in cheese, enteric coated bread, muffin, cake, pasta, various sauces, candy bars, as an anticaking agent for cheese, excipient adsorbent for candy bars, etc. The bulk specific gravity of the powder is 0.25g/cm3The angle of repose was 49.2 °.
The physical property data of the powdered cellulose samples of the above examples 1 and comparative examples were measured, and compared as follows:
Example 2
A method for producing powdery cellulose comprises the following steps:
raw materials: industrial grade wood pulp: content of α -cellulose: 88.13 percent; ash content: 0.15 percent; loss on drying: 7.9 percent; polymerization degree: 1137.
hydrochloric acid: total acidity: 31 percent; reduction product: < 0.007%.
1. 1500kg of deionized water was added to a 2000L enamel reactor, the stirrer was started, and 2.5kg of concentrated hydrochloric acid (about 31% by mass) was slowly added to prepare a 0.05% diluted hydrochloric acid solution. Adding 500kg of industrial wood pulp slowly into a 4000L novel double-shaft differential high-shear reaction device, starting a spacer steam heating switch, and injecting a prepared dilute hydrochloric acid solution. Industrial-grade wood pulp is swelled, mixed and depolymerized in a novel double-shaft differential high-shear horizontal reaction kettle to prepare a wood pulp mixture with the solid content of 24.5%, and the wood pulp mixture is heated to 67 ℃ and is continuously depolymerized for 1.5 hours under the condition of heat preservation.
2. Keeping the temperature for continuous depolymerization to obtain a crude cellulose product, observing an aqueous dispersion solution with the solid content of 1% by using a microscope, depolymerizing the cellulose from a bulk state to a long fiber state, obviously shortening the fiber length, and detecting the polymerization degree 587.
3. Stopping heating after depolymerization, stirring to obtain a slurry material, diluting the slurry material with water until the content is about 10%, pulping for 2 hours by using a vertical three-stage high-speed high-shear cellulose refining dispersion machine, pumping the obtained slurry into a plate-and-frame filter press for filter pressing, rinsing with deionized water to be neutral to obtain a cellulose crude product with the solid content of 46.1%, and obtaining a filter cake wet material of 973.9kg, wherein the yield is 97.5% (calculated on dry products). The cellulose is dried by a high shear granulation dryer.
4. Drying at the air inlet temperature of 150 ℃ and 200 ℃ and the air outlet temperature of 70-80 ℃ in the high-shear granulation drying device.
5. Crushing: the depolymerized cellulose was pulverized into powder by a pulverizer dedicated for cellulose micronization in a combination of various forms of grinding, shearing and collision, and passed through a 400-mesh screen. The powdered cellulose product had a loss on drying of 3.7% and a weight of 445.3kg, a yield of 95.5% (on a dry basis), a laser particle size of D10=6.82 μm, D50=16.19 μm, D90=30.64 μm, and a 400 mesh sieve passage rate of 100%.
Comparative materials: superfine coating additive powdery cellulose BE600-10TG
BE600-10TG is a powdery additive for chemical building material products, which is prepared by treating wood pulp, is a water-insoluble natural fiber, and has excellent flexibility strength, dispersibility and chemical inertness. Produced by JRS, regen mell cellulose, germany. It is suitable for emulsion paint and dry powder coating, and the dry powder is added with 0.1-0.3% to obtain the fiber fruit increasing and thickening effects of the product; improved thixotropy and resistance to flow and improved stability; enhancing the shrinkage resistance and crack resistance; the operation time is prolonged. The strength of the latex paint can be enhanced and improved by adding 0.5-3.0% into the latex paint; the stability and the scrubbing resistance of the emulsion paint are improved, the water retention of the emulsion paint is improved, the tension of a paint film is reduced, and the cracking phenomenon is reduced; the operability is improved, and the splashing phenomenon during rolling and brushing is reduced; reducing the surface gloss. The laser particle size is D10=6.9 μm, D50=16.6 μm, D90=34.22 μm, and the passing rate of a 400-mesh sieve is 99%.
The physical property data of the powdered cellulose samples of the above example 2 and comparative example were measured, and compared as follows:
as can BE seen from Table 2, the main physical property indexes of the powdery cellulose of the coating additive prepared by the invention are that the laser particle size distribution of the powdery cellulose of example 2 is slightly smaller than that of German BE600-10TG, and the fineness of 400 meshes is close to that of German BE600-10 TG. The detection indexes of the powdery cellulose produced by the method in the embodiment 2 all reach or exceed the international level, and the blank of domestic products is filled. Different types of products which can meet the market demand can be produced by adjusting the process parameters.
Compared with the national standard of food additives and the physicochemical indexes of Chinese pharmacopoeia, the powdery cellulose prepared by the method meets the following standards.
The structure of the pulverizer special for cellulose micronization used in the embodiment is shown in figure 1, and comprises a feeding part 01, a pulverizing part 02 communicated with the feeding part 01 and a classifying part 03 communicated with the pulverizing part 02, wherein the feeding part 01 is provided with a feeding hole A, and the classifying part 03 is provided with a discharging hole B.
The feeding part 01 is shown in the attached figure 2 and comprises a feeding bin 11, an outlet of the feeding bin 11 is communicated with the crushing part 02, and a feeding rotating wheel 12 which is driven by a motor to rotate and transversely arranged is arranged in the feeding bin 11, as shown in the attached figure 3. As the material is fibrous, the conventional blade structure is easy to cause the dead locking, so that the outer end part of the runner blade 121 of the feeding runner 12 is provided with a conical structure, and the edge is provided with sawteeth, as shown in figures 3 and 4, so as to reduce the resistance of cellulose and effectively solve the problem of the motor shutdown caused by the motor damage caused by the dead locking of the blade.
The crushing component 02 comprises a crushing box 21 and a crushing structure arranged in the crushing box 21, wherein the crushing structure comprises a main shaft 22, an auxiliary shaft 23 arranged around the main shaft 22 and a grinding wheel 24 arranged on the auxiliary shaft 23, and a blade is arranged on the outer surface of the grinding wheel 24 and spirally arranged along the axial direction of the grinding wheel 24. The main shaft 22 is driven by the motor 04 to rotate, the upper end of the main shaft 22 is provided with a rotor frame 25, the auxiliary shaft 23 is mounted on the rotor frame 25 to drive the rotor frame 25 to rotate, and the auxiliary shaft 23 also rotates along with the rotor frame 25. The gap between the grinding wheel 24 and the inner wall of the crushing box 21 is not more than 1.5 cm. In this way, a grinding zone is formed between the grinding wheel 24 and the inner wall of the crushing box 21, and the material in the grinding zone is sufficiently ground during the continuous rotation of the grinding wheel 24. The grinding wheels 24 are rotatably connected to the auxiliary shafts 23, and when the main shaft 22 rotates, the grinding wheels 24 not only revolve around the main shaft 22, but also rotate around the respective auxiliary shafts 23, so that the grinding, shearing and colliding effects are simultaneously achieved, and the cellulose crushing effect is improved. The lower surface of the rotor frame 25 is provided with a scraper structure, the scraper structure comprises a scraper shaft arranged on the rotor frame 25 and a scraper arranged at the front end of the scraper shaft, the scraper is positioned below the grinding wheel 24, and in the synchronous rotating process of the scraper and the grinding wheel 24, materials are scraped and thrown into a grinding area formed by the grinding wheel 24 and the inner wall of the box to form a padding material layer, and the material layer is crushed by the centrifugal force (namely, extrusion force) inside and outside the material layer generated by the rotation of the grinding wheel 24, so that the effect of refining cellulose is achieved.
The grinding wheel 24 generates strong centrifugal force in the process of revolution and autogyration, strong roller grinding action is generated between the grinding wheel and the stator, the crushed materials enter a grinding area formed by the grinding wheel 24 and the stator under the driving of the centrifugal force and a rotating force field of the grinding wheel 24, and the materials are crushed under the action of strong extrusion force and grinding force. The spiral cutter gap on the grinding wheel 24 can be adjusted according to the fineness requirement of the product, so that powdered cellulose products with different models can be produced.
The classification component 03 comprises a classification box 31 arranged above the crushing box 21 and a classification disc 32 arranged in the classification box 31, a discharge hole B connected with a suction device is arranged above the classification disc 32, and an air inlet is further formed in the crushing box 21. The structure of the grading plate 32 is shown in figure 6, and different types of powdered cellulose can be produced by adjusting the fineness of the product according to the rotating speed of the grading plate 32.
Claims (10)
1. A method for producing powdery cellulose is characterized by comprising the following steps:
s1, adding a low-concentration hydrochloric acid solution into wood pulp, and preserving heat for 1.5 to 2 hours at the temperature of 60 to 80 ℃ to obtain a slurry material; the mass concentration of the hydrochloric acid solution is 0.03-0.05%;
s2, performing filter pressing on the slurry material, and collecting a filter cake;
s3, drying the filter cake;
and S4, crushing the dried filter cake to obtain powdery cellulose.
2. The method for producing powdery cellulose according to claim 1, wherein the solid content of the wood pulp is controlled to 20 to 25% by adding the hydrochloric acid solution.
3. The method for producing powdery cellulose according to claim 1, wherein the filter cake in the step (S2) is washed with clear water to be neutral.
4. The method for producing powdered cellulose according to claim 1, wherein the treatment with the hydrochloric acid solution of the same concentration is repeated once after the step (S1), and the temperature is 20 to 40 ℃.
5. The method for producing powdery cellulose according to claim 1, wherein the pulverization in the step (S4) employs a pulverizer dedicated for micronization of cellulose, the pulverizer comprising: the device comprises a feeding part, a crushing part communicated with the feeding part and a grading part communicated with the crushing part, wherein the feeding part is provided with a feeding hole, and the grading part is provided with a discharging hole; the feeding part comprises a feeding bin, an outlet of the feeding bin is communicated with the crushing part, and a feeding rotating wheel which is driven by a motor to rotate and is transversely arranged is arranged in the feeding bin.
6. The method for producing powdery cellulose according to claim 5, wherein the edge of the runner blade of the feed runner is provided with serrations.
7. A method for producing powdery cellulose according to claim 5 or 6, wherein the outer end portion of the runner blade of the feed runner is tapered.
8. The method according to claim 5, wherein the pulverization member comprises a pulverization chamber, a pulverization structure provided in the pulverization chamber, and a main shaft rotated by a motor, an auxiliary shaft provided around the main shaft, and a grinding wheel provided on the auxiliary shaft.
9. The method for producing powdered cellulose according to claim 8, wherein the clearance between said grinding wheel and the inner wall of said pulverization chamber is not more than 1.5 cm.
10. The method according to claim 8, wherein the classifying means comprises a classifying box disposed above the pulverizing box, and a classifying tray disposed in the classifying box, wherein a discharge port connected to a suction device is disposed above the classifying tray, and an air inlet is further disposed on the pulverizing box.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110847794.5A CN113417164A (en) | 2021-07-27 | 2021-07-27 | Production method of powdery cellulose |
| PCT/CN2021/132286 WO2023005074A1 (en) | 2021-07-27 | 2021-11-23 | Method for producing powdered cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110847794.5A CN113417164A (en) | 2021-07-27 | 2021-07-27 | Production method of powdery cellulose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113417164A true CN113417164A (en) | 2021-09-21 |
Family
ID=77718348
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110847794.5A Pending CN113417164A (en) | 2021-07-27 | 2021-07-27 | Production method of powdery cellulose |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN113417164A (en) |
| WO (1) | WO2023005074A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114982903A (en) * | 2022-05-18 | 2022-09-02 | 江西诺泰生物科技有限公司 | Rice pulp moderate hydrolysis device for producing infant nutrition rice flour |
| WO2023005074A1 (en) * | 2021-07-27 | 2023-02-02 | 湖州市菱湖新望化学有限公司 | Method for producing powdered cellulose |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117654136B (en) * | 2024-02-01 | 2024-04-02 | 天津骏琳科技有限责任公司 | Self-cleaning recovery device for paper support packaging production wastewater |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202590918U (en) * | 2012-05-11 | 2012-12-12 | 新疆光大山河化工科技有限公司 | Efficient micro pulverizer for producing cellulose ether |
| CN103087204A (en) * | 2011-10-28 | 2013-05-08 | 上海同化新材料科技有限公司 | Micro-powder cellulose preparation method |
| CN204710523U (en) * | 2015-06-10 | 2015-10-21 | 嵊州市联丰粉碎设备有限公司 | A kind ofly be applied to the ultra-fine wood powder producing machine grinding processing |
| CN109021120A (en) * | 2018-05-28 | 2018-12-18 | 河南科高辐射化工科技有限公司 | A kind of microcrystalline cellulose environment-friendly preparation method thereof based on mechanochemistry acidolysis technology |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2338196A (en) * | 1941-02-18 | 1944-01-04 | Du Pont | Production of viscose |
| GB554838A (en) * | 1942-01-17 | 1943-07-21 | British United Shoe Machinery | Improvements in or relating to methods of obtaining industrially useful products from material, preferably scrap or waste material, comprising a fibrous base charged with a cellulose derivative or to products which may be obtained from such material |
| CA1180698A (en) * | 1981-12-18 | 1985-01-08 | Jerome B. Thompson | Process for preparing cellulose and product therefrom |
| AU2001267860B2 (en) * | 2000-07-05 | 2005-06-16 | Asahi Kasei Kabushiki Kaisha | Cellulose powder |
| CN107413438A (en) * | 2017-08-30 | 2017-12-01 | 郑州大学 | One kind is used for capsule powder and prepares medicine powder lapping device |
| CN109137591A (en) * | 2018-09-20 | 2019-01-04 | 上海同化新材料科技有限公司 | It is used to prepare the device of powdered cellulose |
| CN113417164A (en) * | 2021-07-27 | 2021-09-21 | 湖州市菱湖新望化学有限公司 | Production method of powdery cellulose |
-
2021
- 2021-07-27 CN CN202110847794.5A patent/CN113417164A/en active Pending
- 2021-11-23 WO PCT/CN2021/132286 patent/WO2023005074A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087204A (en) * | 2011-10-28 | 2013-05-08 | 上海同化新材料科技有限公司 | Micro-powder cellulose preparation method |
| CN202590918U (en) * | 2012-05-11 | 2012-12-12 | 新疆光大山河化工科技有限公司 | Efficient micro pulverizer for producing cellulose ether |
| CN204710523U (en) * | 2015-06-10 | 2015-10-21 | 嵊州市联丰粉碎设备有限公司 | A kind ofly be applied to the ultra-fine wood powder producing machine grinding processing |
| CN109021120A (en) * | 2018-05-28 | 2018-12-18 | 河南科高辐射化工科技有限公司 | A kind of microcrystalline cellulose environment-friendly preparation method thereof based on mechanochemistry acidolysis technology |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023005074A1 (en) * | 2021-07-27 | 2023-02-02 | 湖州市菱湖新望化学有限公司 | Method for producing powdered cellulose |
| CN114982903A (en) * | 2022-05-18 | 2022-09-02 | 江西诺泰生物科技有限公司 | Rice pulp moderate hydrolysis device for producing infant nutrition rice flour |
| CN114982903B (en) * | 2022-05-18 | 2023-04-18 | 江西诺泰生物科技有限公司 | Rice pulp moderate hydrolysis device for producing infant nutrition rice flour |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2023005074A1 (en) | 2023-02-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113417164A (en) | Production method of powdery cellulose | |
| CN101070352B (en) | Method for preparing sheet-like microcrystal cellulose and modification processing method | |
| US9447199B2 (en) | Method for extracting brown algae polysaccharide via microwave chemical process | |
| EP2225387B1 (en) | Process for producing saccharide | |
| CN102813147B (en) | Preparation method of jujube residue insoluble dietary fiber powder | |
| CN103271308B (en) | High-transparency konjaku flour preparation method | |
| Zhao et al. | Extracting xylooligosaccharides in wheat bran by screening and cellulase assisted enzymatic hydrolysis | |
| CN112121917A (en) | Energy-saving efficient biomass fiber separation device | |
| JP5943489B2 (en) | Pretreatment method of raw material for hydrolysis reaction of plant biomass and saccharification method of plant biomass | |
| CN109320618A (en) | A kind of method that extrusion collaboration alkaline process improves cereals starch extraction rate | |
| CN109021120A (en) | A kind of microcrystalline cellulose environment-friendly preparation method thereof based on mechanochemistry acidolysis technology | |
| CN113208120A (en) | Preparation method and application of Pickering emulsifying nano citrus peel dietary fiber | |
| CN107243402A (en) | A kind of disintegrating process of dehydrated vegetables | |
| Liu et al. | Nitrocellulose | |
| CN215997035U (en) | Crushing apparatus for producing powdery cellulose | |
| CN103087204B (en) | Micro-powder cellulose preparation method | |
| CN113372458B (en) | Spherical nanocellulose and green macro preparation method and application thereof | |
| WO2014007295A1 (en) | Method for decomposing plant biomass, and method for producing glucose | |
| JP2012170355A (en) | Method for saccharifying woody biomass | |
| CN109054045A (en) | Preparation method of submicron lignin | |
| CN1051093C (en) | Manufacture of nm avicel powder by solvent process | |
| JP6431756B2 (en) | Biomass component separation method | |
| CN114378912B (en) | Preparation method of bamboo cellulose | |
| CN111500461B (en) | Wall breaking method of haematococcus pluvialis | |
| CN113966347B (en) | Structuring agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |