WO2023005074A1 - Method for producing powdered cellulose - Google Patents
Method for producing powdered cellulose Download PDFInfo
- Publication number
- WO2023005074A1 WO2023005074A1 PCT/CN2021/132286 CN2021132286W WO2023005074A1 WO 2023005074 A1 WO2023005074 A1 WO 2023005074A1 CN 2021132286 W CN2021132286 W CN 2021132286W WO 2023005074 A1 WO2023005074 A1 WO 2023005074A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cellulose
- crushing
- powdered cellulose
- feeding
- hydrochloric acid
- Prior art date
Links
- 239000001913 cellulose Substances 0.000 title claims abstract description 128
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229920003124 powdered cellulose Polymers 0.000 title claims abstract description 35
- 235000019814 powdered cellulose Nutrition 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 235000010980 cellulose Nutrition 0.000 claims abstract description 93
- 229920002678 cellulose Polymers 0.000 claims abstract description 93
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 24
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000012065 filter cake Substances 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims description 42
- 238000010298 pulverizing process Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 22
- 239000000835 fiber Substances 0.000 abstract description 16
- 238000006116 polymerization reaction Methods 0.000 abstract description 15
- 230000009471 action Effects 0.000 abstract description 12
- 229920000642 polymer Polymers 0.000 abstract description 4
- 150000007522 mineralic acids Chemical class 0.000 abstract description 3
- 230000036314 physical performance Effects 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 26
- 238000000034 method Methods 0.000 description 14
- 239000000843 powder Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 238000005903 acid hydrolysis reaction Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 230000005484 gravity Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000003973 paint Substances 0.000 description 6
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- 239000004816 latex Substances 0.000 description 5
- 229920000126 latex Polymers 0.000 description 5
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 5
- 239000008108 microcrystalline cellulose Substances 0.000 description 5
- 229940016286 microcrystalline cellulose Drugs 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000009478 high shear granulation Methods 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000010009 beating Methods 0.000 description 3
- 235000013373 food additive Nutrition 0.000 description 3
- 239000002778 food additive Substances 0.000 description 3
- 238000011085 pressure filtration Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 206010016807 Fluid retention Diseases 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 235000013351 cheese Nutrition 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 102220042174 rs141655687 Human genes 0.000 description 2
- 102220076495 rs200649587 Human genes 0.000 description 2
- 102220043159 rs587780996 Human genes 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 235000012970 cakes Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 235000012459 muffins Nutrition 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 235000015927 pasta Nutrition 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 235000013580 sausages Nutrition 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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
Definitions
- the invention belongs to the field of polymer compound preparation, and relates to a method for preparing cellulose, in particular to a method for producing powdered cellulose.
- Cellulose is the oldest and most abundant natural polymer on the earth. It is inexhaustible and the most precious natural renewable resource for human beings. Cellulose is the most widely distributed and most abundant polysaccharide in nature, accounting for more than 50% of the carbon content in the plant kingdom. The cellulose content of cotton is close to 100%, making it the purest natural source of cellulose. In general wood, cellulose accounts for 40-50%, and there are 10-30% hemicellulose and 20-30% lignin. Cellulose is a substance that cannot be digested and absorbed by humans, but it plays an important role in ensuring human health and prolonging life. It is called the seventh nutrient.
- Cellulose is a lumpy substance with poor fluidity and less exposure of surface hydroxyl groups, which is not conducive to its application. It is necessary to prepare cellulose from a lumpy form to a powder form to endow cellulose with new functions. Through technical research, powdered cellulose products of different shapes and types are produced, with different fineness, bulk specific gravity, fiber length, particle size and particle size, ranging from fine powder or firm particles with good fluidity to coarse and fluffy, It is imperative to meet the needs of cellulose in different application fields in a non-fluid form.
- the microstructure of powdered cellulose is ribbon-like curved, uneven, porous, and flat at the intersections. It has good toughness, dispersibility and chemical stability, and strong water absorption capacity. Therefore, it is widely used in pharmaceuticals, food, cosmetics and industries.
- the field has a wide range of applications, and can be used in construction, electric power, oil processing, metallurgy, chemical fiber, printing and dyeing, filter materials, friction materials, gaskets, environmental protection, sewage treatment, seawater desalination, sulfonate refining, etc. Widely used in concrete, mortar, gypsum products, wood pulp sponge, asphalt roads and other fields, to prevent coating cracking, improve water retention, improve production stability and construction suitability, increase strength, and enhance surface adhesion Wait for good results.
- the powdered cellulose developed in China is not as good as foreign products in terms of product color, average fiber length, water-soluble content, heavy metal content and other major indicators.
- Pharmaceutical grade, food grade and even industrial grade high-end powdered cellulose have high quality requirements.
- the powdered cellulose used in China is basically imported from Germany, the United States, Japan and other countries.
- Well-known foreign companies include Solvira Specialties Inc of the United States, Jeluwerk of Germany FMK Company and German JRS Ruidenmeier Cellulose Company, although the quality is better, but the price is high.
- the present invention provides a production method of powdery cellulose, and obtains powdery cellulose with all indicators meeting the powdery cellulose standard and better fluidity white.
- the present invention adopts following technical scheme:
- a method for producing powdery cellulose comprising the steps of:
- the above technical solution adopts the production process of first partially depolymerizing cellulose through the action of chemical energy and then pulverizing it with mechanical energy to obtain powdery cellulose.
- the fiber is hydrolyzed with an extremely low concentration of inorganic acid, and the cellulose polymer is partially depolymerized by controlling a certain degree of polymerization.
- the cellulose is partially degraded by the action of chemical energy, the length of the molecular chain is shortened by the action of chemical energy, the strength of the cellulose is reduced, and it is easier to be crushed by mechanical energy, so that powdered cellulose with different grades of physical properties can be prepared.
- the cellulose that is partially degraded by chemical energy is reduced in molecular chain length and fiber strength, and then it is mechanically pulverized, and it is easier to be pulverized by mechanical energy into finer-grained and better fluidity powdered cellulose.
- the invention breaks the inertial thinking, and controls the degree of polymerization of cellulose by adjusting the acid hydrolysis process conditions and using a very low concentration hydrochloric acid solution.
- the degree of polymerization ⁇ 500 is powdery cellulose. If the acid concentration is too high, the temperature is too high, the hydrolysis speed is too fast, and the reaction process is difficult to control, resulting in excessive acid hydrolysis, which may degrade into microcrystalline cellulose and lose the characteristics of the target product powdery cellulose; if the acid concentration is too low, the temperature If it is too low and the reaction speed is too slow, the toughness of cellulose cannot be reduced and the subsequent mechanical crushing process will be affected.
- Process research Control the concentration of hydrochloric acid at 0.03-0.05%, and control the acid hydrolysis reaction temperature at 60-80°C for acid hydrolysis test, the best acid hydrolysis effect can be obtained.
- the solid content of the wood pulp is controlled to be 20 to 25%.
- the filter cake in step (S2) is washed to neutral with clean water.
- the treatment is repeated once with a hydrochloric acid solution of the same concentration at a temperature of 20 to 40°C.
- the first acidolysis is carried out at a higher temperature, which is beneficial to the depolymerization of cellulose, and then repeat the acidolysis at a lower temperature.
- the molecular movement in the solution slows down, and the degree of polymerization of powdered cellulose does not meet the requirements.
- Cellulose with longer molecular chains continues to depolymerize, while cellulose that reaches the required degree of polymerization will not continue to be depolymerized into microcrystalline cellulose. Ensure that the degree of polymerization of powdered cellulose is still maintained under acid treatment conditions.
- the pulpy material is subjected to beating treatment, so that it is easier to be pulverized, pulverized and ground into a finer particle size and a higher bulk specific gravity. Larger, better flowing powdered cellulose product.
- the principle of this method is that after the cellulose is partially degraded by the action of chemical energy, the length of the molecular chain is shortened by the action of chemical energy, and the strength of the cellulose is reduced. shaped cellulose.
- the pulverization in step (S4) is pulverized into powder by a special pulverizer for cellulose miniaturization through grinding, shearing and collision.
- the pulverizer includes: a feeding part, a pulverizing part connected with the feeding part, a classification part connected with the pulverizing part, the feeding part is provided with a feeding port, and the classification part is provided with a discharge mouth.
- the feeding part includes a feeding bin, an outlet of the feeding bin communicates with the crushing part, and a horizontally arranged feeding wheel driven by a motor is arranged inside the feeding bin.
- the edges of the runner blades of the feed runner are provided with serrations.
- the outer ends of the runner blades of the feed runner have a conical structure.
- the crushing component includes a crushing box, a crushing structure arranged in the crushing box, the crushing structure includes a main shaft, an auxiliary shaft arranged around the main shaft, and a grinding wheel arranged on the auxiliary shaft, the main shaft is composed of The motor is driven to rotate, and the auxiliary shaft is driven to rotate by the main shaft.
- the gap between the grinding wheel and the inner wall of the crushing box is no more than 1.5 cm.
- a grinding zone is formed between the grinding wheel and the inner wall of the crushing box, and the materials in the grinding zone are fully ground during the continuous rotation of the grinding wheel.
- the grinding wheels are rotatably connected to the auxiliary shaft.
- the grinding wheels When the main shaft rotates, the grinding wheels not only revolve around the main shaft, but also rotate around their respective auxiliary shafts. This process has grinding, shearing, collision The effect of improving the crushing effect of cellulose.
- blades are provided on the outer surface of the grinding wheel, and the blades are helically arranged along the axial direction of the grinding wheel.
- the upper end of the main shaft is provided with a rotor frame, and the auxiliary shaft is mounted on the rotor frame.
- a scraper structure is provided on the lower surface of the rotor frame, and the scraper structure includes a scraper shaft arranged on the rotor frame and a scraper arranged at the front end of the scraper shaft, and the scraper is located below the grinding wheel.
- the grading component includes a grading box arranged above the crushing box, a grading disk arranged in the grading box, an outlet connected with a suction device is arranged above the grading disk, and the crushing box There is also an air inlet.
- the fineness of the product is adjusted according to the rotating speed of the classifying disc, so that different types of powdered cellulose can be produced.
- the grinding wheel Through the centrifugal force of the grinding wheel, it continuously grinds, shears and collides with the pulverizer in a three-in-one movement, so that the cellulose is crushed and sheared in both horizontal and vertical directions to improve the crushing efficiency, which can make the fineness of powdered cellulose finer and the bulk specific gravity. Larger powders have better fluidity, and different types of products that can meet market demand can be produced by adjusting process parameters.
- the present invention has the following advantages:
- the fiber is hydrolyzed with an extremely low concentration of inorganic acid, and the cellulose polymer is partially depolymerized by controlling a certain degree of polymerization.
- the length of the molecular chain is shortened by the action of chemical energy, the strength of the cellulose is reduced, and it is easier to be crushed by mechanical energy to obtain powdered cellulose with different grades of physical properties.
- the pulverizer in the present invention through the centrifugal force of the grinding wheel, continues to grind, shear and collide with the pulverizer in a trinity movement, so that the cellulose is crushed and sheared in the horizontal and vertical directions to improve the pulverization efficiency, and the powdery fiber can be made
- the fineness of the powder is finer, the bulk specific gravity is larger, and the fluidity of the powder is better.
- Raw materials food grade wood pulp: ⁇ -cellulose content: 96.8%; ash content: 0.06%; loss on drying: 7.8%; degree of polymerization: 1073.
- Hydrochloric acid total acidity: 31%; reducing substances: ⁇ 0.007%.
- the air inlet temperature is 150-200°C and the outlet air temperature is 70-80°C for drying.
- Pulverization The depolymerized cellulose is pulverized into powder through a combination of grinding, shearing and collision with a special pulverizer for cellulose miniaturization. After passing through a 60-mesh sieve, the powdered cellulose product has a weight loss on drying of 3.9%, the weight is 449.8kg, the yield is 95.7% (calculated as dry product), the bulk specific gravity is 0.26g/cm3, and the angle of repose is 47.1°.
- Comparative material Food additive powdered cellulose JustFiber BH200
- JustFiber BH200 is a purified cellulose-containing plant fiber pulp obtained by processing ⁇ -cellulose. It has a large bulk density and good fluidity as a powdery cellulose. It is manufactured by Solvaira International Cellulose Corporation (IFC), North Tonawanda, New York, USA. Produced by Specialties Inc. It is used in the food industry as a dietary fiber, resists sticking or as a carrier material, and has a high chemical and microbiological purity. It is an ingredient that is odorless and tasteless and can effectively reduce the calorie content in food. It does not contain calories, fat, or digestible carbohydrates.
- Example 1 As can be seen from Table 1, the main physical performance indicators of the food additive powdery cellulose prepared by the present invention, the bulk specific gravity of Example 1 is slightly greater than that of U.S. JustFiber BH200, and the angle of repose is higher than that of U.S. JustFiber BH200. The BH200 is lower, indicating that the fluidity of the powder is better.
- the powdery cellulose produced by the present invention in Example 1 has all the detection indexes reaching or leading the international level, filling the blank of domestic products. By adjusting the process parameters, different models can be produced to meet the market demand.
- Raw materials Industrial grade wood pulp: ⁇ -cellulose content: 88.13%; Ash content: 0.15%; Loss on drying: 7.9%; Polymerization degree: 1137.
- Hydrochloric acid total acidity: 31%; reducing substances: ⁇ 0.007%.
- the air inlet temperature is 150-200°C and the outlet air temperature is 70-80°C for drying.
- Pulverization The depolymerized cellulose is pulverized into powder through a combination of grinding, shearing and collision with a special pulverizer for cellulose miniaturization, and passes through a 400-mesh sieve.
- the powdered cellulose product has a loss on drying of 3.7%, a weight of 445.3kg, and a yield of 95.5% (calculated as a dry product).
- Comparative material Superfine coating additive powdered cellulose BE600-10TG
- the coating additive powdery cellulose main physical performance index prepared by the present invention, embodiment 2 laser particle size distribution is slightly finer than Germany BE600-10TG, 400 mesh sieve fineness and Germany BE600-10TG near.
- the powdery cellulose produced by the present invention in Example 2 has all the detection indexes reaching or leading the international level, filling the blank of domestic products. By adjusting the process parameters, different models can be produced to meet the market demand.
- the special pulverizer for cellulose miniaturization used in the examples has a structure as shown in Figure 1, including a feeding part 01, a pulverizing part 02 connected with the feeding part 01, and a pulverizing part connected with the pulverizing part 02.
- a grading component 03, the feeding component 01 is provided with an inlet A, and the grading component 03 is provided with an outlet B.
- the feeding part 01 includes a feeding bin 11, the outlet of the feeding bin 11 is connected to the pulverizing part 02, and the feeding bin 11 is provided with a lateral arrangement driven by a motor to rotate.
- the crushing component 02 includes a crushing box 21, a crushing structure arranged in the crushing box 21, the crushing structure includes 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 , the outer surface of the grinding wheel 24 is provided with blades, and the blades are helically arranged along the axial direction of the grinding wheel 24 .
- the main shaft 22 is driven to rotate by the motor 04, and the upper end of the main shaft 22 is provided with a rotor frame 25, and 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 thereupon.
- the gap between the grinding wheel 24 and the inner wall of the crushing box 21 is no more than 1.5 cm.
- a grinding zone is formed between the grinding wheel 24 and the inner wall of the crushing box 21, and the materials in the grinding zone are fully ground during the continuous rotation of the grinding wheel 24.
- the grinding wheel 24 is rotatably connected to the auxiliary shaft 23.
- the main shaft 22 rotates, the grinding wheel 24 not only revolves around the main shaft 22, but also rotates around the respective auxiliary shaft 23. This process has grinding, shearing, The effect of collision improves the crushing effect of cellulose.
- the lower surface of the rotor frame 25 is provided with a scraper structure, the scraper structure includes a scraper shaft arranged on the rotor frame 25 and a scraper arranged at the front end of the scraper shaft, the scraper is located below the grinding wheel 24, During the synchronous rotation of the scraper and the grinding wheel 24, the material is scraped and thrown into the grinding area formed by the grinding wheel 24 and the inner wall of the box to form a pad layer. The material is crushed, that is, the effect of cellulose micronization is achieved.
- the grinding wheel 24 produces a strong centrifugal force during the revolution and self-propagation, and has a strong roller grinding effect with the stator. Driven by the centrifugal force and the rotating force field of the grinding wheel 24, the crushed materials enter the grinding area formed by the grinding wheel 24 and the stator. The material is crushed under the action of strong extrusion force and grinding force. It is also possible to adjust the clearance of the spiral knife on the grinding wheel 24 according to the fineness of the product, so as to produce different types of powdered cellulose products.
- the grading unit 03 includes a grading box 31 arranged above the crushing box 21, a grading disk 32 arranged in the grading box 31, a discharge port B connected with a suction device is arranged above the grading disk 32,
- the crushing box 21 is also provided with an air inlet.
- the structure of the classifying disc 32 is shown in Figure 6, and the fineness of the product can be adjusted according to the rotating speed of the classifying disc 32, so that different types of powdered cellulose can be produced.
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
A method for producing powdered cellulose, which comprises following steps: S1, adding a low-concentration hydrochloric acid solution into wood pulp, and keeping the temperature at 60-80ºC for 1.5-2 hours to obtain a slurry material, wherein the mass concentration of the hydrochloric acid solution is 0.03-0.05%; S2, subjecting the slurry material to filter pressing, and collecting a filter cake; S3, drying the filter cake; and S4, crushing the dried filter cake to obtain powdered cellulose. The powdered cellulose is prepared by means of a production process of partial depolymerization of cellulose under the action of chemical energy and then crushing same by means of mechanical energy. The fibers are hydrolyzed by an inorganic acid with extremely low concentration, and the cellulose polymer is partially depolymerized by means of controlling a certain degree of polymerization. After the cellulose is partially depolymerized under 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, such that the powdered cellulose with different grades of physical performance indexes is obtained.
Description
本发明属于高分子化合物制备领域,涉及一种纤维素制备方法,尤其是一种粉状纤维素的生产方法。The invention belongs to the field of polymer compound preparation, and relates to a method for preparing cellulose, in particular to a method for producing powdered cellulose.
纤维素是地球上最古老、最丰富的天然高分子,是取之不尽用之不竭的,是人类最宝贵的天然可再生资源。纤维素是自然界中分布最广、含量最多的一种多糖,占植物界碳含量的50%以上。棉花的纤维素含量接近100%,为天然的最纯纤维素来源。一般木材中,纤维素占40~50%,还有10~30%的半纤维素和20~30%的木质素。纤维素是一种不被人类消化吸收的物质,但是在保障人类健康,延长生命方面有着重要作用,称它为第七种营养素。Cellulose is the oldest and most abundant natural polymer on the earth. It is inexhaustible and the most precious natural renewable resource for human beings. Cellulose is the most widely distributed and most abundant polysaccharide in nature, accounting for more than 50% of the carbon content in the plant kingdom. The cellulose content of cotton is close to 100%, making it the purest natural source of cellulose. In general wood, cellulose accounts for 40-50%, and there are 10-30% hemicellulose and 20-30% lignin. Cellulose is a substance that cannot be digested and absorbed by humans, but it plays an important role in ensuring human health and prolonging life. It is called the seventh nutrient.
纤维素为团状物质,流动性差,表面羟基暴露少,不利于对其进行应用,必须将纤维素从团状制备为粉状形态从而赋予纤维素新的功能。通过技术研究生产出不同形态不同型号的粉状纤维素产品,以细度、堆比重、纤维长度、颗粒度、粒径大小不同,从流动性良好的细粉或结实的颗粒到粗且蓬松、无流动性的形态,以满足不同应用领域对纤维素的使用需求是当务之急。Cellulose is a lumpy substance with poor fluidity and less exposure of surface hydroxyl groups, which is not conducive to its application. It is necessary to prepare cellulose from a lumpy form to a powder form to endow cellulose with new functions. Through technical research, powdered cellulose products of different shapes and types are produced, with different fineness, bulk specific gravity, fiber length, particle size and particle size, ranging from fine powder or firm particles with good fluidity to coarse and fluffy, It is imperative to meet the needs of cellulose in different application fields in a non-fluid form.
粉状纤维素微观结构是带状弯曲的,凹凸不平的,多孔的,交叉处是扁平的,有良好的韧性、分散性和化学稳定性,吸水能力强,因此在制药、食品、化妆品和工业领域具有广泛应用,可运用于建筑、电力、油品加工、冶金、化纤、印染、过滤材料、摩擦材料、密封垫、环境保护、污水处理、海水淡化、磺酸盐精制等方面。广泛用于混凝土、砂浆、石膏制品、木浆海棉、沥青道路等领域,对防止涂层开裂、提高保水性、提高生产的稳定性和施工的合宜性、增加强度、增强对表面的附着力等有良好的效果。The microstructure of powdered cellulose is ribbon-like curved, uneven, porous, and flat at the intersections. It has good toughness, dispersibility and chemical stability, and strong water absorption capacity. Therefore, it is widely used in pharmaceuticals, food, cosmetics and industries. The field has a wide range of applications, and can be used in construction, electric power, oil processing, metallurgy, chemical fiber, printing and dyeing, filter materials, friction materials, gaskets, environmental protection, sewage treatment, seawater desalination, sulfonate refining, etc. Widely used in concrete, mortar, gypsum products, wood pulp sponge, asphalt roads and other fields, to prevent coating cracking, improve water retention, improve production stability and construction suitability, increase strength, and enhance surface adhesion Wait for good results.
目前市场上由国内研制的粉状纤维素,无论在产品色泽、纤维平均长度、水溶物含量、重金属含量等主要指标上均不如国外产品。医药级、食品级甚至工业级高端粉状纤维素质量要求高,现在国内使用的粉状纤维素基本上都是从德国、美国、日本等国家进口,国外知名企业有美国Solvira Specialties Inc、德国Jeluwerk FMK公司、德国JRS瑞登梅尔纤维素公司,虽然质量较好,但价位高。我国规模以上粉状纤维素生产企业几乎没有。At present, the powdered cellulose developed in China is not as good as foreign products in terms of product color, average fiber length, water-soluble content, heavy metal content and other major indicators. Pharmaceutical grade, food grade and even industrial grade high-end powdered cellulose have high quality requirements. The powdered cellulose used in China is basically imported from Germany, the United States, Japan and other countries. Well-known foreign companies include Solvira Specialties Inc of the United States, Jeluwerk of Germany FMK Company and German JRS Ruidenmeier Cellulose Company, although the quality is better, but the price is high. There are almost no powdery cellulose production enterprises above designated size in my country.
国内在团状纤维素深加工起步较晚,只有简单的破碎,产品堆比重轻、粒径粗、流动性差,使用范围受到限制。目前国内外研究和生产粉状纤维素的主要生产工艺是使用机械粉碎法,即通过机械力粉碎降低纤维素粒径,将净化的纤维素浆转化成粉状纤维素。此工艺存在明显缺陷:由于纤维之间连接强度高,在制备过程中需要多次粉碎,多次研磨,机械能耗高、成本高,并且生产的粉状纤维素粒径相对比较粗。因此,如何简单高效地解决以上技术难关,开发研究生产粉状纤维素的新工艺方法,并形成产业化生产,具有重要的社会和经济意义。The deep processing of lumpy cellulose started late in China, and only simple crushing is required. The product has a light bulk specific gravity, coarse particle size, and poor fluidity, so the scope of use is limited. At present, the main production process of research and production of powdered cellulose at home and abroad is to use mechanical pulverization, that is, to reduce the particle size of cellulose through mechanical pulverization, and convert the purified cellulose pulp into powdered cellulose. This process has obvious defects: due to the high connection strength between the fibers, multiple crushing and grinding are required in the preparation process, high mechanical energy consumption and high cost, and the particle size of the produced powdery cellulose is relatively coarse. Therefore, it is of great social and economic significance to solve the above technical difficulties simply and efficiently, to develop and research a new process for producing powdery cellulose, and to form industrialized production.
本发明为了克服现有技术中粉状纤维素制备存在的上述缺陷,提供一种粉状纤维素的生产方法,获得各项指标均满足粉状纤维素标准,且流动性更好的粉状纤维素。In order to overcome the above-mentioned defects in the preparation of powdery cellulose in the prior art, the present invention provides a production method of powdery cellulose, and obtains powdery cellulose with all indicators meeting the powdery cellulose standard and better fluidity white.
本发明采用如下的技术方案:The present invention adopts following technical scheme:
一种粉状纤维素的生产方法,包括如下步骤:A method for producing powdery cellulose, comprising the steps of:
S1.向木浆中加入低浓度的盐酸溶液,在温度为60至80℃条件下保温1.5至2小时,得到浆状物料;所述盐酸溶液的质量浓度为0.03至0.05%;S1. Add low-concentration hydrochloric acid solution to the wood pulp, and keep it warm for 1.5 to 2 hours at a temperature of 60 to 80° C. to obtain a pulpy material; the mass concentration of the hydrochloric acid solution is 0.03 to 0.05%;
S2.将所述浆状物料进行压滤,收集滤饼;S2. Press-filter the slurry material to collect the filter cake;
S3.干燥所述滤饼;S3. drying the filter cake;
S4.粉碎干燥后的滤饼,得到粉状纤维素。S4. Pulverize the dried filter cake to obtain powdery cellulose.
上述技术方案采用先通过化学能作用对纤维素进行部分解聚再使用机械能粉碎制备得到粉状纤维素的生产工艺。通过极低浓度无机酸水解纤维,控制一定聚合度部分解聚纤维素聚合物。纤维素经化学能作用部分降解后,受到化学能的作用分子链长度缩短,纤维素强度降低,更容易被机械能粉碎,可以制备得到不同等级物理性能指标的粉状纤维素。经化学能作用部分降解的纤维素由于分子链的长度降低,纤维强度降低,再对其进行机械粉碎,而更容易被机械能粉碎成更细粒度、流动性更好的粉状纤维素。The above technical solution adopts the production process of first partially depolymerizing cellulose through the action of chemical energy and then pulverizing it with mechanical energy to obtain powdery cellulose. The fiber is hydrolyzed with an extremely low concentration of inorganic acid, and the cellulose polymer is partially depolymerized by controlling a certain degree of polymerization. After the cellulose is partially degraded by the action of chemical energy, the length of the molecular chain is shortened by the action of chemical energy, the strength of the cellulose is reduced, and it is easier to be crushed by mechanical energy, so that powdered cellulose with different grades of physical properties can be prepared. The cellulose that is partially degraded by chemical energy is reduced in molecular chain length and fiber strength, and then it is mechanically pulverized, and it is easier to be pulverized by mechanical energy into finer-grained and better fluidity powdered cellulose.
现有技术中,只有在制备微晶纤维素才采用酸解,按照本领域的常规理解,采用酸解无法获得粉状纤维素,而是获得聚合度更低的微晶纤维素。In the prior art, acid hydrolysis is only used in the preparation of microcrystalline cellulose. According to the conventional understanding in the field, powdered cellulose cannot be obtained by acid hydrolysis, but microcrystalline cellulose with a lower degree of polymerization.
本发明打破惯性思维,通过调整酸解工艺条件,采用极低浓度的盐酸溶液,来控制纤维素聚合度,一般聚合度≥500为粉状纤维素。若酸浓度过高,温度过高,水解速度太快,反应过程难以控制,造成过度酸解,可能降解为微晶纤维素会失去目标产品粉状纤维素的特性;若酸浓度太低,温度太低,反应速度太慢,则不能降低纤维素的韧性,影响后续的机械粉碎加工。工艺研究将盐酸浓度控制在0.03-0.05%,酸解反应温度控制在60-80℃进行酸解试验,可取得最佳的酸解效果。The invention breaks the inertial thinking, and controls the degree of polymerization of cellulose by adjusting the acid hydrolysis process conditions and using a very low concentration hydrochloric acid solution. Generally, the degree of polymerization ≥ 500 is powdery cellulose. If the acid concentration is too high, the temperature is too high, the hydrolysis speed is too fast, and the reaction process is difficult to control, resulting in excessive acid hydrolysis, which may degrade into microcrystalline cellulose and lose the characteristics of the target product powdery cellulose; if the acid concentration is too low, the temperature If it is too low and the reaction speed is too slow, the toughness of cellulose cannot be reduced and the subsequent mechanical crushing process will be affected. Process research Control the concentration of hydrochloric acid at 0.03-0.05%, and control the acid hydrolysis reaction temperature at 60-80°C for acid hydrolysis test, the best acid hydrolysis effect can be obtained.
而且在此盐酸浓度之内,即使酸解时间过长,纤维素仍然不会被过度酸解而成为微晶纤维素,申请人做了相关实验,在盐酸浓度0.03%,温度75℃下,分别酸解2h、4h、6h、8h、10h,对应的聚合度为591、573、562、550、541,仍然满足粉状纤维素聚合度要求。Moreover, within this hydrochloric acid concentration, even if the acid hydrolysis time is too long, the cellulose will not be excessively acid hydrolyzed and become microcrystalline cellulose. The applicant has done related experiments. After acid hydrolysis for 2h, 4h, 6h, 8h, and 10h, the corresponding degrees of polymerization are 591, 573, 562, 550, and 541, which still meet the requirements for the degree of polymerization of powdered cellulose.
作为优选,加入盐酸溶液后控制木浆的固含量为20至25%。Preferably, after adding the hydrochloric acid solution, the solid content of the wood pulp is controlled to be 20 to 25%.
作为优选,采用清水对步骤(S2)中滤饼进行清洗至中性。Preferably, the filter cake in step (S2) is washed to neutral with clean water.
作为优选,在步骤(S1)之后,采用相同浓度的盐酸溶液重复处理一次,温度为20至40℃。第一次酸解在较高温度下进行,有利于纤维素的解聚,之后再在较低温度下重复酸解,此时溶液内分子活动减慢,未达到粉状纤维素聚合度要求的较长分子链的纤维素继续解聚,而达到聚合度要求的纤维素则不会继续被解聚成为微晶纤维素。确保在酸处理条件下,仍然保持粉状纤维素的聚合度。Preferably, after the step (S1), the treatment is repeated once with a hydrochloric acid solution of the same concentration at a temperature of 20 to 40°C. The first acidolysis is carried out at a higher temperature, which is beneficial to the depolymerization of cellulose, and then repeat the acidolysis at a lower temperature. At this time, the molecular movement in the solution slows down, and the degree of polymerization of powdered cellulose does not meet the requirements. Cellulose with longer molecular chains continues to depolymerize, while cellulose that reaches the required degree of polymerization will not continue to be depolymerized into microcrystalline cellulose. Ensure that the degree of polymerization of powdered cellulose is still maintained under acid treatment conditions.
作为优选,在酸解之后,压滤之前(也即在步骤S1与步骤S2之间),对浆状物料进行打浆处理,从而更容易被粉碎细化、粉碎研磨成粒度更细、堆比重更大、流动性更好的粉状纤维素产品。此方法原理在于纤维素经化学能作用部分降解后,受到化学能的作用分子链长度缩短,纤维素强度降低,更容易被机械能粉碎细化、粉碎研磨,可以制备得到不同等级物理性能指标的粉状纤维素。 Preferably, after the acid hydrolysis, before the pressure filtration (that is, between step S1 and step S2), the pulpy material is subjected to beating treatment, so that it is easier to be pulverized, pulverized and ground into a finer particle size and a higher bulk specific gravity. Larger, better flowing powdered cellulose product. The principle of this method is that after the cellulose is partially degraded by the action of chemical energy, the length of the molecular chain is shortened by the action of chemical energy, and the strength of the cellulose is reduced. shaped cellulose.
作为优选,步骤(S4)中粉碎采用通过纤维素微细化专用粉碎机,通过研磨、剪切、碰撞多种形式结合的方式粉碎成粉末。Preferably, the pulverization in step (S4) is pulverized into powder by a special pulverizer for cellulose miniaturization through grinding, shearing and collision.
该粉碎机包括:进料部件、与所述进料部件相连通的粉碎部件、与所述粉碎部件相连通的分级部件,所述进料部件设置进料口,所述分级部件设置有出料口。The pulverizer includes: a feeding part, a pulverizing part connected with the feeding part, a classification part connected with the pulverizing part, the feeding part is provided with a feeding port, and the classification part is provided with a discharge mouth.
作为优选,所述进料部件包括进料仓,所述进料仓的出口连通所述粉碎部件,所述进料仓内设置有由电机带动转动的横向设置的进料转轮。Preferably, the feeding part includes a feeding bin, an outlet of the feeding bin communicates with the crushing part, and a horizontally arranged feeding wheel driven by a motor is arranged inside the feeding bin.
作为优选,所述进料转轮的转轮叶片的边缘设置有锯齿。Preferably, the edges of the runner blades of the feed runner are provided with serrations.
作为优选,所述进料转轮的转轮叶片的外端部呈锥形结构。Preferably, the outer ends of the runner blades of the feed runner have a conical structure.
作为优选,所述粉碎部件包括粉碎箱、设置于粉碎箱内的粉碎结构,所述粉碎结构包括主轴、围绕所述主轴设置的辅轴以及设置于所述辅轴上的磨轮,所述主轴由电机带动转动,所述辅轴由所述主轴带动转动。Preferably, the crushing component includes a crushing box, a crushing structure arranged in the crushing box, the crushing structure includes a main shaft, an auxiliary shaft arranged around the main shaft, and a grinding wheel arranged on the auxiliary shaft, the main shaft is composed of The motor is driven to rotate, and the auxiliary shaft is driven to rotate by the main shaft.
作为优选,所述磨轮与所述粉碎箱的内壁之间的间隙不超过1.5cm。这样,磨轮与粉碎箱的内壁之间形成研磨区,在磨轮不断转动的过程中,研磨区物料受到充分研磨。Preferably, the gap between the grinding wheel and the inner wall of the crushing box is no more than 1.5 cm. In this way, a grinding zone is formed between the grinding wheel and the inner wall of the crushing box, and the materials in the grinding zone are fully ground during the continuous rotation of the grinding wheel.
作为优选,所述磨轮转动连接于所述辅轴,在所述主轴转动时,所述磨轮不仅围绕主轴进行公转,同时又围绕各自的辅轴进行自转,此过程同时具有研磨、剪切、碰撞的作用,提高了纤维素的粉碎效果。Preferably, the grinding wheels are rotatably connected to the auxiliary shaft. When the main shaft rotates, the grinding wheels not only revolve around the main shaft, but also rotate around their respective auxiliary shafts. This process has grinding, shearing, collision The effect of improving the crushing effect of cellulose.
作为优选,所述磨轮的外表面设置有刀片,所述刀片沿着所述磨轮轴向螺旋设置。Preferably, blades are provided on the outer surface of the grinding wheel, and the blades are helically arranged along the axial direction of the grinding wheel.
作为优选,所述主轴的上端设置有转子架,所述辅轴安装于所述转子架上。Preferably, the upper end of the main shaft is provided with a rotor frame, and the auxiliary shaft is mounted on the rotor frame.
作为优选,所述转子架的下表面设置有刮刀结构,所述刮刀结构包括设置于所述转子架上的刮刀轴和设置于所述刮刀轴前端的刮刀,所述刮刀位于所述磨轮下方。Preferably, a scraper structure is provided on the lower surface of the rotor frame, and the scraper structure includes a scraper shaft arranged on the rotor frame and a scraper arranged at the front end of the scraper shaft, and the scraper is located below the grinding wheel.
作为优选,所述分级部件包括设置于所述粉碎箱上方的分级箱、设置于所述分级箱内的分级盘,所述分级盘上方设置有连有吸引装置的出料口,所述粉碎箱上还设置有进风口。Preferably, the grading component includes a grading box arranged above the crushing box, a grading disk arranged in the grading box, an outlet connected with a suction device is arranged above the grading disk, and the crushing box There is also an air inlet.
作为优选,沿着粉状纤维素的出料口方向,根据分级盘转速来调节产品细度,可生产出不同型号的粉状纤维素。As a preference, along the direction of the discharge port of the powdered cellulose, the fineness of the product is adjusted according to the rotating speed of the classifying disc, so that different types of powdered cellulose can be produced.
通过磨轮的离心力,持续与粉碎机研磨、剪切和碰撞三位一体运动,使纤维素在横向和竖向都进行破碎和剪切提高粉碎效率,可使粉状纤维素的细度更细、堆比重更大、粉体的流动性更好,通过调整工艺参数可生产出不同型号能满足市场需求的产品。Through the centrifugal force of the grinding wheel, it continuously grinds, shears and collides with the pulverizer in a three-in-one movement, so that the cellulose is crushed and sheared in both horizontal and vertical directions to improve the crushing efficiency, which can make the fineness of powdered cellulose finer and the bulk specific gravity. Larger powders have better fluidity, and different types of products that can meet market demand can be produced by adjusting process parameters.
通过实施上述技术方案,相比现有技术,本发明具有如下的优点:By implementing the above technical scheme, compared with the prior art, the present invention has the following advantages:
1.采用先通过化学能作用对纤维素进行部分解聚再使用机械能粉碎制备得到粉状纤维素的生产工艺。通过极低浓度无机酸水解纤维,控制一定聚合度部分解聚纤维素聚合物。纤维素经化学能作用部分降解后,受到化学能的作用分子链长度缩短,纤维素强度降低,更容易被机械能粉碎,得到不同等级物理性能指标的粉状纤维素。1. Adopt the production process of firstly depolymerizing the cellulose partially through the action of chemical energy and then pulverizing it with mechanical energy to obtain powdery cellulose. The fiber is hydrolyzed with an extremely low concentration of inorganic acid, and the cellulose polymer is partially depolymerized by controlling a certain degree of polymerization. After the cellulose is partially degraded by the action of chemical energy, the length of the molecular chain is shortened by the action of chemical energy, the strength of the cellulose is reduced, and it is easier to be crushed by mechanical energy to obtain powdered cellulose with different grades of physical properties.
2.相比现有技术中纯机械粉碎,制造成本更低。2. Compared with pure mechanical crushing in the prior art, the manufacturing cost is lower.
3.本发明中的粉碎机,通过磨轮的离心力,持续与粉碎机研磨、剪切和碰撞三位一体运动,使纤维素在横向和竖向都进行破碎和剪切提高粉碎效率,可使粉状纤维素的细度更细、堆比重更大、粉体的流动性更好,通过调整工艺参数可生产出不同型号能满足市场需求的产品。3. The pulverizer in the present invention, through the centrifugal force of the grinding wheel, continues to grind, shear and collide with the pulverizer in a trinity movement, so that the cellulose is crushed and sheared in the horizontal and vertical directions to improve the pulverization efficiency, and the powdery fiber can be made The fineness of the powder is finer, the bulk specific gravity is larger, and the fluidity of the powder is better. By adjusting the process parameters, different models can be produced to meet the market demand.
附图1为本发明一实施例所示粉碎机的结构示意图;Accompanying drawing 1 is the structural representation of pulverizer shown in an embodiment of the present invention;
附图2为本发明一实施例所示粉碎机的进料部件的结构示意图;Accompanying drawing 2 is the structural representation of the feeding part of pulverizer shown in an embodiment of the present invention;
附图3为本发明一实施例所示粉碎机的进料转轮的结构示意图;Accompanying drawing 3 is the structural representation of the feed runner of pulverizer shown in one embodiment of the present invention;
附图4为本发明一实施例所示粉碎机的转轮叶片的结构示意图Accompanying drawing 4 is the structural representation of the runner blade of pulverizer shown in one embodiment of the present invention
附图5为本发明一实施例所示粉碎机的粉碎部件的结构示意图;Accompanying drawing 5 is the structural representation of the pulverizing part of pulverizer shown in one embodiment of the present invention;
附图6为本发明一实施例所示粉碎机的的分级盘的结构示意图。Accompanying drawing 6 is the structure diagram of the classifying disk of the pulverizer shown in one embodiment of the present invention.
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明的保护范围。The following clearly and completely describes the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1:Example 1:
一种粉状纤维素的生产方法:A kind of production method of powdery cellulose:
原料:食品级木浆:α-纤维素含量:96.8%;灰分:0.06%;干燥失重:7.8%;聚合度:1073。Raw materials: food grade wood pulp: α-cellulose content: 96.8%; ash content: 0.06%; loss on drying: 7.8%; degree of polymerization: 1073.
盐酸:总酸度:31%;还原物:<0.007%。Hydrochloric acid: total acidity: 31%; reducing substances: <0.007%.
1、在2000L搪瓷反应釜中加入1500kg去离子水,启动搅拌浆,缓慢加入1.5kg浓盐酸(质量分数约为31%),配成0.03%稀盐酸溶液。将500kg食品级木浆慢慢加入4000L新型双轴差速高剪切反应装置,开启隔套蒸汽加热开关,同时将配制好的稀盐酸溶液注入。木浆在新型双轴差速高剪切卧式反应釜中溶胀混合、剪切解聚,制备成固含量24.8%木浆混合物,加热升温至75℃,保温持续解聚2小时。1. Add 1500kg of deionized water to the 2000L enamel reaction kettle, start the stirring paddle, slowly add 1.5kg of concentrated hydrochloric acid (mass fraction is about 31%), and make a 0.03% dilute hydrochloric acid solution. Slowly add 500kg of food-grade wood pulp into the 4000L new biaxial differential high-shear reaction device, turn on the steam heating switch of the spacer, and inject the prepared dilute hydrochloric acid solution at the same time. The wood pulp was swollen, mixed, and sheared and depolymerized in a new type of biaxial differential high-shear horizontal reactor to prepare a wood pulp mixture with a solid content of 24.8%, heated to 75°C, and kept for 2 hours for depolymerization.
2、保温持续解聚后得到纤维素粗品,用显微镜观察固含量1%的水分散溶液,纤维素从团状解聚,变为长纤维状,纤维长度明显变短,并检测聚合度为589。2. Obtain the crude cellulose product after heat preservation and continuous depolymerization. Use a microscope to observe the water dispersion solution with a solid content of 1%. The cellulose depolymerizes from agglomerate to long fiber. The fiber length is obviously shortened, and the degree of polymerization is detected to be 589. .
3、解聚完成后停止加热,搅拌得到浆状物料,对浆状物料加水稀释至含量10%左右使用立式三级高速高剪切纤维素细化分散机进行打浆处理1小时,得到的浆液打入板框压滤机内压滤,用去离子水漂洗至中性,得纤维素粗品固含量45.8%,滤饼湿料共986.2kg,得率97.98%(以干品计)。通过高剪切造粒干燥装置,对纤维素进行干燥。3. After the depolymerization is completed, stop heating, stir to obtain a slurry material, add water to dilute the slurry material to a content of about 10%, and use a vertical three-stage high-speed high-shear cellulose refining disperser for beating treatment for 1 hour to obtain a slurry Put it into a plate and frame filter press for pressure filtration, rinse with deionized water until neutral, and obtain a crude cellulose product with a solid content of 45.8%, and a total of 986.2kg of filter cake wet material, with a yield of 97.98% (calculated as a dry product). The cellulose is dried by a high shear granulation drying device.
4、在高剪切造粒干燥装置进风温度150-200℃,出风温度70-80℃进行干燥。4. In the high-shear granulation drying device, the air inlet temperature is 150-200°C and the outlet air temperature is 70-80°C for drying.
5、粉碎:通过纤维素微细化专用粉碎机对解聚后的纤维素通过研磨、剪切、碰撞多种形式结合的方式粉碎成粉末,通过60目筛网,粉状纤维素产品干燥失重为3.9%,重量为449.8kg,得率95.7%(以干品计),其堆比重为0.26g/cm3,休止角为47.1°。5. Pulverization: The depolymerized cellulose is pulverized into powder through a combination of grinding, shearing and collision with a special pulverizer for cellulose miniaturization. After passing through a 60-mesh sieve, the powdered cellulose product has a weight loss on drying of 3.9%, the weight is 449.8kg, the yield is 95.7% (calculated as dry product), the bulk specific gravity is 0.26g/cm3, and the angle of repose is 47.1°.
比较材料:食品添加剂粉状纤维素JustFiber BH200Comparative material: Food additive powdered cellulose JustFiber BH200
JustFiber BH200是通过处理α-纤维素得到的一种纯化的可从含纤维素的植物的纤维浆制得的,堆比重大、流动性好的粉状纤维素。其由美国纽约州北托纳旺达市的国际纤维素公司(IFC)Solvaira
Specialties Inc生产。其用于食品行业作为膳食纤维,具有抗粘结或起载体材料的作用,并具有高的化学和微生物纯度。是一种无臭无味并能有效减少食品中热量的含量的一种成分,不含热量、脂肪、没有可消化的碳水化合物。可以应用于乳酪、肠衣面包、松饼、蛋糕、意大利面、各类调味酱、压片糖果,作为乳酪抗结剂、压片糖果赋形剂吸附剂等等。其堆比重为0.25g/cm3,休止角为49.2°。JustFiber BH200 is a purified cellulose-containing plant fiber pulp obtained by processing α-cellulose. It has a large bulk density and good fluidity as a powdery cellulose. It is manufactured by Solvaira International Cellulose Corporation (IFC), North Tonawanda, New York, USA.
Produced by Specialties Inc. It is used in the food industry as a dietary fiber, resists sticking or as a carrier material, and has a high chemical and microbiological purity. It is an ingredient that is odorless and tasteless and can effectively reduce the calorie content in food. It does not contain calories, fat, or digestible carbohydrates. It can be used in cheese, sausage casing bread, muffins, cakes, pasta, various sauces, tableted candy, as an anti-caking agent for cheese, as an excipient adsorbent for tableted candy, etc. Its bulk specific gravity is 0.25g/cm3, and its angle of repose is 49.2°.
检测上述实施例1、比较例的粉状纤维素试样的物理性能数据,对照比较如下:Detect the physical property data of the powdery cellulose sample of above-mentioned embodiment 1, comparative example, contrast is as follows:
从表1中可以看出,通过本发明制备得到的食品添加剂粉状纤维素主要物理性能指标,实施例1堆比重稍大于美国JustFiber BH200、休止角比美国JustFiber
BH200更低,说明粉体的流动性更好。本发明生产的粉状纤维素实施例1各项检测指标均达到或领先于国际水平,填补国内产品空白。通过调整工艺参数可生产出不同型号能满足市场需求的产品。As can be seen from Table 1, the main physical performance indicators of the food additive powdery cellulose prepared by the present invention, the bulk specific gravity of Example 1 is slightly greater than that of U.S. JustFiber BH200, and the angle of repose is higher than that of U.S. JustFiber BH200.
The BH200 is lower, indicating that the fluidity of the powder is better. The powdery cellulose produced by the present invention in Example 1 has all the detection indexes reaching or leading the international level, filling the blank of domestic products. By adjusting the process parameters, different models can be produced to meet the market demand.
实施例2Example 2
一种粉状纤维素的生产方法:A kind of production method of powdery cellulose:
原料:工业级木浆:α-纤维素含量:88.13%;灰分:0.15%;干燥失重:7.9%;聚合度:1137。Raw materials: Industrial grade wood pulp: α-cellulose content: 88.13%; Ash content: 0.15%; Loss on drying: 7.9%; Polymerization degree: 1137.
盐酸:总酸度:31%;还原物:<0.007%。Hydrochloric acid: total acidity: 31%; reducing substances: <0.007%.
1、在2000L搪瓷反应釜中加入1500kg去离子水,启动搅拌浆,缓慢加入2.5kg浓盐酸(质量分数约为31%),配成0.05%稀盐酸溶液。将500kg工业级木浆慢慢加入4000L新型双轴差速高剪切反应装置,开启隔套蒸汽加热开关,同时将配制好的稀盐酸溶液注入。工业级木浆在新型双轴差速高剪切卧式反应釜中溶胀混合、剪切解聚,制备成固含量24.5%木浆混合物,加热升温至67℃,保温持续解聚1.5小时。1. Add 1500kg of deionized water into the 2000L enamel reaction kettle, start the stirring paddle, slowly add 2.5kg of concentrated hydrochloric acid (mass fraction is about 31%), and make a 0.05% dilute hydrochloric acid solution. Slowly add 500kg of industrial-grade wood pulp into a 4000L new biaxial differential high-shear reaction device, turn on the steam heating switch of the spacer, and inject the prepared dilute hydrochloric acid solution at the same time. Industrial-grade wood pulp was swollen, mixed, sheared and depolymerized in a new type of biaxial differential speed high-shear horizontal reactor to prepare a wood pulp mixture with a solid content of 24.5%, heated to 67°C, and kept warm for 1.5 hours for continuous depolymerization.
2、保温持续解聚后得到纤维素粗品,用显微镜观察固含量1%的水分散溶液,纤维素从团状解聚,变为长纤维状,纤维长度明显变短,并检测聚合度587。2. Obtain the crude cellulose product after heat preservation and continuous depolymerization. Use a microscope to observe the water dispersion solution with a solid content of 1%. The cellulose depolymerizes from agglomerate to long fiber. The fiber length is obviously shortened, and the degree of polymerization is detected to be 587.
3、解聚完成后停止加热,搅拌得到浆状物料,对浆状物料加水稀释至含量10%左右使用立式三级高速高剪切纤维素细化分散机进行打浆处理2小时,得到的浆液打入板框压滤机内压滤,用去离子水漂洗至中性,得纤维素粗品固含量46.1%,滤饼湿料973.9kg,得率为97.5%(以干品计)。通过高剪切造粒干燥装置,对纤维素进行干燥。3. After the depolymerization is completed, stop heating, stir to obtain a slurry material, add water to dilute the slurry material to a content of about 10%, and use a vertical three-stage high-speed high-shear cellulose refining disperser for beating for 2 hours to obtain a slurry Put it into a plate-and-frame filter press for pressure filtration, rinse with deionized water until neutral, and obtain a crude cellulose product with a solid content of 46.1%, and a filter cake wet material of 973.9kg, with a yield of 97.5% (calculated as a dry product). The cellulose is dried by a high shear granulation drying device.
4、在高剪切造粒干燥装置进风温度150-200℃,出风温度70-80℃进行干燥。4. In the high-shear granulation drying device, the air inlet temperature is 150-200°C and the outlet air temperature is 70-80°C for drying.
5、粉碎:通过纤维素微细化专用粉碎机对解聚后的纤维素通过研磨、剪切、碰撞多种形式结合的方式粉碎成粉末,通过400目筛网。粉状纤维素产品干燥失重为3.7%,重量为445.3kg,得率95.5%(以干品计),其激光粒度为D10=6.82μm、D50=16.19μm、D90=30.64μm,400目筛通过率100% 。5. Pulverization: The depolymerized cellulose is pulverized into powder through a combination of grinding, shearing and collision with a special pulverizer for cellulose miniaturization, and passes through a 400-mesh sieve. The powdered cellulose product has a loss on drying of 3.7%, a weight of 445.3kg, and a yield of 95.5% (calculated as a dry product). The laser particle size is D10=6.82μm, D50=16.19μm, D90=30.64μm, and passed through a 400-mesh sieve. Rate 100%.
比较材料:超细涂料添加剂粉状纤维素BE600-10TGComparative material: Superfine coating additive powdered cellulose BE600-10TG
BE600-10TG是木浆经过处理而制成的用于化学建筑材料产品的粉状添加剂,它是不溶于水的天然纤维,具有优良的柔韧强度、分散性和化学惰性。其由德国瑞登梅尔纤维素公司JRS生产。其适用于乳胶漆和干粉涂料,在干粉料中添加0.1-0.3%可以获得产品的纤维增果和增稠作用;提高触变性和抗流性提高稳定性;增强抗收缩和抗开裂性能;延长操作时间。在乳胶漆中添加0.5-3.0%可以增强和改善乳胶漆的强度;提高乳胶漆稳定性和耐擦洗性,提高乳胶漆保水性,减少漆膜张力,减少开裂现象;改进操作性,减少滚刷时的飞溅现象;减少表面光泽度。其激光粒度为D10=6.9μm、D50=16.6μm、D90=34.22μm,400目筛通过率99%。BE600-10TG is a powdered additive for chemical building material products made from wood pulp. It is a water-insoluble natural fiber with excellent flexibility, strength, dispersibility and chemical inertness. It is produced by JRS, the German Riddenmeier Cellulose Company. It is suitable for latex paint and dry powder coating. Adding 0.1-0.3% to the dry powder can increase the fiber and thicken the product; improve thixotropy and flow resistance to improve stability; enhance shrinkage and crack resistance; prolong operating time. Adding 0.5-3.0% to latex paint can enhance and improve the strength of latex paint; improve the stability and scrub resistance of latex paint, improve the water retention of latex paint, reduce the tension of paint film, and reduce cracking; improve operability and reduce rolling brush Splash phenomenon; reduce surface gloss. Its laser particle size is D10=6.9μm, D50=16.6μm, D90=34.22μm, and the passing rate of 400 mesh sieve is 99%.
检测上述实施例2、比较例的粉状纤维素试样的物理性能数据,对照比较如下:Detect the physical property data of the powdery cellulose sample of above-mentioned embodiment 2, comparative example, contrast is as follows:
从表2中可以看出,通过本发明制备得到的涂料添加剂粉状纤维素主要物理性能指标,实施例2激光粒度分布比德国BE600-10TG稍细、400目筛分细度与德国BE600-10TG接近。本发明生产的粉状纤维素实施例2各项检测指标均达到或领先于国际水平,填补国内产品空白。通过调整工艺参数可生产出不同型号能满足市场需求的产品。As can be seen from Table 2, the coating additive powdery cellulose main physical performance index prepared by the present invention, embodiment 2 laser particle size distribution is slightly finer than Germany BE600-10TG, 400 mesh sieve fineness and Germany BE600-10TG near. The powdery cellulose produced by the present invention in Example 2 has all the detection indexes reaching or leading the international level, filling the blank of domestic products. By adjusting the process parameters, different models can be produced to meet the market demand.
对比食品添加剂国标及中国药典理化指标,本发明制备得到的粉状纤维素均符合以下标准。Comparing the national standards of food additives and the physical and chemical indicators of the Chinese Pharmacopoeia, the powdery cellulose prepared by the present invention all meet the following standards.
实施例中所用的纤维素微细化专用粉碎机,结构如附图1所示,包括进料部件01、与所述进料部件01相连通的粉碎部件02、与所述粉碎部件02相连通的分级部件03,所述进料部件01设置进料口A,所述分级部件03设置有出料口B。The special pulverizer for cellulose miniaturization used in the examples has a structure as shown in Figure 1, including a feeding part 01, a pulverizing part 02 connected with the feeding part 01, and a pulverizing part connected with the pulverizing part 02. A grading component 03, the feeding component 01 is provided with an inlet A, and the grading component 03 is provided with an outlet B.
所述进料部件01如附图2所示,包括进料仓11,所述进料仓11的出口连通所述粉碎部件02,所述进料仓11内设置有由电机带动转动的横向设置的进料转轮12,如附图3所示。由于物料是纤维状,常规的叶片结构很容易造成卡死,因此进料转轮12的转轮叶片121的外端部设置成锥形结构、边缘设置有锯齿,如附图3、4所示,以减少纤维素的阻力,能有效解决叶片卡死引起电机损坏而停机的问题。The feeding part 01, as shown in accompanying drawing 2, includes a feeding bin 11, the outlet of the feeding bin 11 is connected to the pulverizing part 02, and the feeding bin 11 is provided with a lateral arrangement driven by a motor to rotate. The feeding runner 12, as shown in accompanying drawing 3. Because the material is fibrous, the conventional blade structure is easy to cause jamming, so the outer end of the runner blade 121 of the feed runner 12 is set in a tapered structure, and the edge is provided with sawtooth, as shown in Figures 3 and 4 , in order to reduce the resistance of cellulose, which can effectively solve the problem of motor damage caused by blade jamming and shutdown.
所述粉碎部件02包括粉碎箱21、设置于粉碎箱21内的粉碎结构,所述粉碎结构包括主轴22、围绕所述主轴22设置的辅轴23以及设置于所述辅轴23上的磨轮24,所述磨轮24的外表面设置有刀片,所述刀片沿着所述磨轮24轴向螺旋设置。所述主轴22由电机04带动转动,所述主轴22的上端设置有转子架25,所述辅轴23安装于所述转子架25上,带动转子架25转动,辅轴23也随之转动。所述磨轮24与所述粉碎箱21的内壁之间的间隙不超过1.5cm。这样,磨轮24与粉碎箱21的内壁之间形成研磨区,在磨轮24不断转动的过程中,研磨区物料受到充分研磨。磨轮24转动连接于所述辅轴23,在所述主轴22转动时,所述磨轮24不仅围绕主轴22进行公转,同时又围绕各自的辅轴23进行自转,此过程同时具有研磨、剪切、碰撞的作用,提高了纤维素的粉碎效果。所述转子架25的下表面设置有刮刀结构,所述刮刀结构包括设置于所述转子架25上的刮刀轴和设置于所述刮刀轴前端的刮刀,所述刮刀位于所述磨轮24下方,刮刀与磨轮24同步旋转过程中,把物料刮抛喂入到磨轮24与箱内壁组成的研磨区中,形成垫料层,该料层受磨轮24旋转产生内外的离心力(即挤压力)将物料碾碎,即由此达到纤维素微细化的效果。The crushing component 02 includes a crushing box 21, a crushing structure arranged in the crushing box 21, the crushing structure includes 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 , the outer surface of the grinding wheel 24 is provided with blades, and the blades are helically arranged along the axial direction of the grinding wheel 24 . The main shaft 22 is driven to rotate by the motor 04, and the upper end of the main shaft 22 is provided with a rotor frame 25, and 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 thereupon. The gap between the grinding wheel 24 and the inner wall of the crushing box 21 is no 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 materials in the grinding zone are fully ground during the continuous rotation of the grinding wheel 24. The grinding wheel 24 is rotatably connected to the auxiliary shaft 23. When the main shaft 22 rotates, the grinding wheel 24 not only revolves around the main shaft 22, but also rotates around the respective auxiliary shaft 23. This process has grinding, shearing, The effect of collision improves the crushing effect of cellulose. The lower surface of the rotor frame 25 is provided with a scraper structure, the scraper structure includes a scraper shaft arranged on the rotor frame 25 and a scraper arranged at the front end of the scraper shaft, the scraper is located below the grinding wheel 24, During the synchronous rotation of the scraper and the grinding wheel 24, the material is scraped and thrown into the grinding area formed by the grinding wheel 24 and the inner wall of the box to form a pad layer. The material is crushed, that is, the effect of cellulose micronization is achieved.
磨轮24在公转和自传的过程中产生强大的离心力,与定子发生强烈的辊研作用,被粉碎的物料在离心力及磨轮24旋转力场的带动下,进入磨轮24与定子组成的研磨区中,在强大的挤压力和研磨力作用下物料被粉碎。还可以根据产品细度要求调整磨轮24上螺旋刀间隙,从而生产出不同型号的粉状纤维素产品。The grinding wheel 24 produces a strong centrifugal force during the revolution and self-propagation, and has a strong roller grinding effect with the stator. Driven by the centrifugal force and the rotating force field of the grinding wheel 24, the crushed materials enter the grinding area formed by the grinding wheel 24 and the stator. The material is crushed under the action of strong extrusion force and grinding force. It is also possible to adjust the clearance of the spiral knife on the grinding wheel 24 according to the fineness of the product, so as to produce different types of powdered cellulose products.
所述分级部件03包括设置于所述粉碎箱21上方的分级箱31、设置于所述分级箱31内的分级盘32,所述分级盘32上方设置有连有吸引装置的出料口B,所述粉碎箱21上还设置有进风口。分级盘32结构如附图6所示,根据分级盘32转速来调节产品细度,可生产出不同型号的粉状纤维素。The grading unit 03 includes a grading box 31 arranged above the crushing box 21, a grading disk 32 arranged in the grading box 31, a discharge port B connected with a suction device is arranged above the grading disk 32, The crushing box 21 is also provided with an air inlet. The structure of the classifying disc 32 is shown in Figure 6, and the fineness of the product can be adjusted according to the rotating speed of the classifying disc 32, so that different types of powdered cellulose can be produced.
Claims (10)
- 一种粉状纤维素的生产方法,其特征在于,包括如下步骤:A kind of production method of powdery cellulose is characterized in that, comprises the steps:S1.向木浆中加入低浓度的盐酸溶液,在温度为60至80℃条件下保温1.5至2小时,得到浆状物料;所述盐酸溶液的质量浓度为0.03至0.05%;S1. Add low-concentration hydrochloric acid solution to the wood pulp, and keep it warm for 1.5 to 2 hours at a temperature of 60 to 80° C. to obtain a pulpy material; the mass concentration of the hydrochloric acid solution is 0.03 to 0.05%;S2.将所述浆状物料进行压滤,收集滤饼;S2. Press-filter the slurry material to collect the filter cake;S3.干燥所述滤饼;S3. drying the filter cake;S4.粉碎干燥后的滤饼,得到粉状纤维素。S4. Pulverize the dried filter cake to obtain powdered cellulose.
- 根据权利要求1所述的一种粉状纤维素的生产方法,其特征在于,加入盐酸溶液后控制木浆的固含量为20至25%。The production method of a kind of powdered cellulose according to claim 1, characterized in that, after adding the hydrochloric acid solution, the solid content of the wood pulp is controlled to be 20 to 25%.
- 根据权利要求1所述的一种粉状纤维素的生产方法,其特征在于,采用清水对步骤(S2)中滤饼进行清洗至中性。The production method of powdery cellulose according to claim 1, characterized in that the filter cake in step (S2) is washed to neutral with clean water.
- 根据权利要求1所述的一种粉状纤维素的生产方法,其特征在于,在步骤(S1)之后,采用相同浓度的盐酸溶液重复处理一次,温度为20至40℃。The production method of powdered cellulose according to claim 1, characterized in that, after step (S1), the same concentration of hydrochloric acid solution is used to repeat the treatment once, and the temperature is 20 to 40°C.
- 根据权利要求1所述的一种粉状纤维素的生产方法,其特征在于,步骤(S4)中粉碎采用通过纤维素微细化专用粉碎机,该粉碎机包括:进料部件、与所述进料部件相连通的粉碎部件、与所述粉碎部件相连通的分级部件,所述进料部件设置进料口,所述分级部件设置有出料口;所述进料部件包括进料仓,所述进料仓的出口连通所述粉碎部件,所述进料仓内设置有由电机带动转动的横向设置的进料转轮。The production method of powdery cellulose according to claim 1, characterized in that, the pulverization in step (S4) adopts a special pulverizer for cellulose micronization, and the pulverizer includes: a feeding part, and the feeding part A crushing part connected with the material part, a classification part connected with the crushing part, the feeding part is provided with a feeding port, and the classifying part is provided with a discharge port; the feeding part includes a feeding bin, the The outlet of the feeding bin is connected to the crushing part, and a horizontally arranged feeding runner driven by a motor is arranged in the feeding bin.
- 根据权利要求5所述的一种粉状纤维素的生产方法,其特征在于,所述进料转轮的转轮叶片的边缘设置有锯齿。The method for producing powdered cellulose according to claim 5, wherein the edge of the runner blade of the feed runner is provided with sawtooth.
- 根据权利要求5或6所述的一种粉状纤维素的生产方法,其特征在于,所述进料转轮的转轮叶片的外端部呈锥形结构。A method for producing powdery cellulose according to claim 5 or 6, characterized in that the outer end of the runner blade of the feed runner is in a conical structure.
- 根据权利要求5所述的一种粉状纤维素的生产方法,其特征在于,所述粉碎部件包括粉碎箱、设置于粉碎箱内的粉碎结构,所述粉碎结构包括主轴、围绕所述主轴设置的辅轴以及设置于所述辅轴上的磨轮,所述主轴由电机带动转动,所述辅轴由所述主轴带动转动。A method for producing powdered cellulose according to claim 5, wherein the crushing component comprises a crushing box and a crushing structure arranged in the crushing box, the crushing structure includes a main shaft, and is arranged around the main shaft. The auxiliary shaft and the grinding wheel arranged on the auxiliary shaft, the main shaft is driven to rotate by the motor, and the auxiliary shaft is driven to rotate by the main shaft.
- 根据权利要求8所述的一种粉状纤维素的生产方法,其特征在于,所述磨轮与所述粉碎箱的内壁之间的间隙不超过1.5cm。A method for producing powdery cellulose according to claim 8, characterized in that the gap between the grinding wheel and the inner wall of the crushing box is no more than 1.5 cm.
- 根据权利要求8所述的一种粉状纤维素的生产方法,其特征在于,所述分级部件包括设置于所述粉碎箱上方的分级箱、设置于所述分级箱内的分级盘,所述分级盘上方设置有连有吸引装置的出料口,所述粉碎箱上还设置有进风口。A method for producing powdery cellulose according to claim 8, wherein the grading components include a grading box arranged above the crushing box, a grading disc arranged in the grading box, and the A discharge port connected with a suction device is arranged above the classifying disc, and an air inlet is also arranged on the crushing box.
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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 |
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