CN102159637A - Cellulose-containing mass - Google Patents
Cellulose-containing mass Download PDFInfo
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- CN102159637A CN102159637A CN2010800034722A CN201080003472A CN102159637A CN 102159637 A CN102159637 A CN 102159637A CN 2010800034722 A CN2010800034722 A CN 2010800034722A CN 201080003472 A CN201080003472 A CN 201080003472A CN 102159637 A CN102159637 A CN 102159637A
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- 239000001913 cellulose Substances 0.000 title claims abstract description 78
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 108010059892 Cellulase Proteins 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 2
- 235000010469 Glycine max Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 235000007319 Avena orientalis Nutrition 0.000 description 1
- 241000209763 Avena sativa Species 0.000 description 1
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- QMGYPNKICQJHLN-UHFFFAOYSA-M Carboxymethylcellulose cellulose carboxymethyl ether Chemical group [Na+].CC([O-])=O.OCC(O)C(O)C(O)C(O)C=O QMGYPNKICQJHLN-UHFFFAOYSA-M 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 101100447328 Corynebacterium glutamicum (strain ATCC 13032 / DSM 20300 / BCRC 11384 / JCM 1318 / LMG 3730 / NCIMB 10025) ftsQ gene Proteins 0.000 description 1
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- 101000925662 Enterobacteria phage PRD1 Endolysin Proteins 0.000 description 1
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 244000046109 Sorghum vulgare var. nervosum Species 0.000 description 1
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- 239000012736 aqueous medium Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
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- 235000011194 food seasoning agent Nutrition 0.000 description 1
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- 239000004571 lime Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
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- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
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- 239000001814 pectin Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/28—Treatment by wave energy or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2397/00—Characterised by the use of lignin-containing materials
- C08J2397/02—Lignocellulosic material, e.g. wood, straw or bagasse
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Paper (AREA)
Abstract
The invention concerns a method for producing a cellulose-containing mass comprising an organic material, the method comprising the steps a) preparation of an input comprising organic material and a liquid content, and b) exposing said input to a wet-mixing procedure at a temperature in the range of 40 to 90 DEG C preferably 50 to 80 DEG C and most preferred around 60 DEG C or exposing said input to an active zone of an electromagnetic field. According to a further embodiment of the present invention, cellulose of different types is added to the input. Moreover a method for producing a composite material that is based on said cellulose-containing mass is disclosed as well as a product produced of said composite material.
Description
Technical field
The present invention relates to method, the matrix material of claim 23 and the product of claim 24 of production matrix material of cellulose material, the claim 18 of method, the claim 17 of the production cellulose material of claim 1.
Described method can be used for multiple practical use.For example, produced the surface layer of New Building Materials, different brightwork, finishing material, interior trim, various high resistance and firmness etc. by the agricultural waste of cereal (for example corn, rye, wheat, oat, barley, Chinese sorghum, rape, rice etc. and binding substances thereof), staple fiber (cotton, flax, hemp etc.), this makes described production suitable economically owing to the low cost that drops into material.
Background technology
Exist at present some for example to be suitable for packing matrix material with the known organic origin of Application in Building.Although xylon is very common, yet also be used as fibrous packing once in a while from other natural fibers of crop or cereal.
US2006043629A proposes by using coupling agent, be that the functional monomer is polymer-modified, handle biological plastics with soya-based and be the natural fiber (for example grass, rice straw, wheat straw, industrial hemp, arghan) of matrix and produce the enhanced biological matrix material.The modified soybean powder that just contains the functional monomer in addition industrial application for example the purposes aspect reactive extrusion molding and the injection molding set forth.
US 2008/181969A has solved and has comprised for example matrix material variable color and structure (i.e. chemistry or the machinery) degraded of xylon, stalk, grass and other organic materialss of cellulosic component that is connected with polymeric constituent by coupling agent.Described coupling agent, for example grafting-maleic anhydride polymkeric substance or multipolymer, have can be at described polymkeric substance and cellulosic component inner or between form the functional group of covalent linkage.
Technical problem
An object of the present invention is to provide improving one's methods of production cellulose material, described cellulose material is provided and the method for the high strength composite of producing the primary structure comprise organic materials---preferred source is from organic materials of higher plant---is provided, described higher plant by in the cell between different piece, functional group, side chain and/or other parts of different polymkeric substance and/or described polymkeric substance and the iuntercellular structure be connected to form its natural form (for example stalk).
Summary of the invention
The present invention relates to high strength composite and multiplely make by cheap organic material; preferably by the stalk of higher plant part, to contain the capacity Mierocrystalline cellulose (be macromolecule polysaccharide or by β-1; the dextran that the D-glucose that 4-connects constitutes) or the production of the article made of the cell walls of chitin (by β-1, the glycan that the N-ethanoyl that 4-connects-D-glucosamine constitutes) or cytolemma.In this application, term cellulose material, drop into material and/or matrix material and also should comprise and contain chitinous material, drop into material and/or mixture, perhaps cellulose with contain chitinous material, drop into the mixture of material and/or matrix material.Mierocrystalline cellulose---modal organic compound on the earth---is that the molecular formula that is configured to the polymer chain of β-glucose unit is [C
6H
7O
2(OH)
3]
nMacromolecule polysaccharide (glycan), wherein the scope of n is from hundreds of to thousands of.The present invention can produce matrix material and need not to use and make for example external source polymeric component that mutually combines of vegetable particle of described organic materials.In the context of the present invention, to refer to described polymeric component be not to come from described organic material to be processed to the term external source.An essential characteristic of the novel method of described production cellulose material is to make described organic materials be exposed to the service area of artificial electromagnetic field.
The novel method that production can be used for producing the cellulose material of the matrix material that is suitable for high-strength products may further comprise the steps at least:
A) preparation comprises the input material of organic materials and liquid contents; With
B) described input is expected in 70 to 120 ℃, preferred 80 to 100 ℃, most preferably the temperature in 92 to 94 ℃ of scopes is carried out wet grinding.
According to embodiment preferred, except that step b) or replacement step b), make described input material be exposed to the service area of artificial electromagnetic field.
According to embodiment preferred, in process of production, drop in the natural form of material and the born of the same parents thereof be connected with intercellular structure organic destroyed, up to generating liquid and/or paste substance.This material is further used as molding sand and uses: it is new geometrical shape by reshaping, and is recovered in the structure connection simultaneously of this paste solidified.The solidified paste becomes the article of final use.
Hereinafter, term " drops into material " and is used to represent to be exposed to the initial substance of electromagnetic field or the mixture of material, and the product that term " cellulose material " expression is produced by aforesaid method of the present invention.Described product is considered to intermediates (being also referred to as the output material), because it is further used for producing multiple product.
The viewpoint of present method is the following fact, and in process of production, the natural form and the born of the same parents' combination interior and the intercellular structure thereof that drop into material are destroyed, up to generating uniform liquid and/or paste substance.This cellulose material is further used as molding sand and uses: it is new geometrical shape by reshaping, and is recovered in the structure connection simultaneously of this paste solidified.The solidified paste becomes the article of final use.
---preferable methyl Mierocrystalline cellulose and/or carboxymethyl cellulose---preferably is added to described cellulose material with the form of sodium salt and/or Microcrystalline Cellulose according to embodiment preferred, with other Mierocrystalline celluloses.According to another preferred embodiment of the present invention, described other Mierocrystalline celluloses to small part adds as the part that contains the concentration of fibre element that produces in the wet grinding process.The cellulosic liquid portion that contains that produces in the wet grinding process or afterwards can be by filtering or dehydration concentrates, till this part reaches required content of cellulose (relevant with water content) level.
In this application, term " organic materials " is understood to include and contains cellulosic any materials.Preferably, the organic materials of input comprises the fiber that has mixed cellulosic molecule.Advantageously, the organic materials that is derived from higher plant preferably is selected from Gramineae (Poaceae) class---for example cereal crop---very grass, perhaps cotton, hemp or flax or its mixture.In at least a or test of its mixture in using grain stem or rice straw, produced good result as described organic materials.
Preferably, described organic materials was reduced to small-particle or or even slurry in preprocessing process before being exposed to electromagnetic field.Preferably the organic materials to described input material carries out preprocessing/pre-treatment, depends on described type of material and condition.These conditions are the per-cent that is used to generate the micellar β-Xian Weisu of ultra-fine protofibril form in the existence, microbe population, pure input material of humidity, cleanliness factor, incoherent natural or manual member.Preliminary determine protofibril and described protofibril aggegation is become the organic constituent content between the Mierocrystalline cellulose of stiff fibre be proved to be favourable.Usually, contain aggegation or become the glue material for example the organic materials of pectin be suitable, but the hydrophobic organic materials that has more that contains soft wood for example or cutin also is suitable.Perhaps also can use the organic materials that contains lignin.The essential characteristic of the product or the article of producing or character can pre-determine by changing these and other mutual relationship of secondary substance in described cellulose material.
The pre-treatment of organic materials comprises dipping, be aided with electromechanics, fluid power and ultrasonic wave effect and boil, the method for decatize and other known processing material of vegetable origin.The notable feature of cellulosic fibre is to have the resistance to fracture that is only second to steel, and the resistance that mechanical effect and physical action are changed.If described organic materials is a stem, the stem of paddy rice or wheat or rye for example, then available pH value be about 8 or higher, be more preferably 8.4 or higher liquid flood, then and/or simultaneously with electromechanics effect, fluid power effect, ultrasonic wave effect, boil, decatize or its combination.
For example WO 08/112191 is known by prior art, and in lignocellulosic biomass, the crystalline cellulose protofibril is embedded in the not too regular hemicellulose matrix, and it is surrounded by the xylogen sealer of outside again.The cellulose materials of natural generation is contacted with lytic enzyme, cause being lower than 20% theory expectation result's cellulose hydrolysis productive rate usually.Therefore, before saccharan (Mierocrystalline cellulose and the hemicellulose) enzymatic hydrolysis of attempting to make in the biomass, to carry out " pre-treatment " to biomass inevitably.Pre-treatment is meant lignocellulosic biomass is converted into the effective form of cellulose hydrolysis from its natural form (it is obstinate for the cellulase system under this form).With compare without pretreated biomass, be characterised in that the surface-area (porosity) that cellulase with increase can touch and the dissolving or the reallocation of xylogen through effective pretreated lignocellulosic materials.The porosity that increases mainly is because the destruction/dissolving of the destruction of cellulose crystallity, hemicellulose and xylogen reallocation and/or dissolved combination cause.In different current pretreatment approaches, realize that the associated efficiency of the described factor of part (or owning) is greatly different.These current pretreatment approaches comprise diluted acid, vapor action, pyrolysis method, " organic solvent " method (needing the participation of the organic solvent in the aqueous medium), ammonia solution filament expansion method (AFEX), highly basic method (using the alkali such as ammonia, NaOH or lime etc.) and the processing of highly enriched phosphoric acid.The method that is contained cellulosic biomaterial by the known method of above-mentioned prior art and other known processing can advantageously combine with method steps of the present invention.
Required character and/or preprocessing process according to described cellulose material (being described input material), exogenous liquid contents---promptly by organic material liquid contents that provide or that be derived from organic material itself---is enough, thereby needn't adds ectogenic or extra liquid.In its simplest embodiment, form described liquid contents by water.Yet other liquid (for example organic solvent) or gas or other fluid can be suitable for as liquid contents, depend on the characteristic to the requirement of throughput and the article that formed by described matrix material afterwards.Yet, importantly, can realize the suitable effect of liquid contents and organic materials.At liquid is not under the situation of water, and the key of the preferred embodiments of the invention is after producing described cellulose material, if necessary, can extract excessive liquid contents with suitable manner.
According to the purposes and the predetermined treatment process of expection, liquid contents preferably comprises solvent, for example is used to make the organic materials maturation.
The process that structure connect to be recovered appears at uniform material in new mould solidified the time; This process is actually n β-glucose molecule residual body and is generally [C to the polymkeric substance formula
6H
7O
2(OH)
3]
nThe integration process of molecular compound.Known have 3 oh groups [(OH) in each residual body
3Group] the existence of glucose molecule make following apparent: be able between each residual body of glucose molecule by lateral oh group and therefrom the elimination of water molecule connect.Therefore, when this material dehydration, recurring structure connects recovery accidentally in uniform substance, and causes its curing.
Test shows that when the input material package that is exposed to the electromagnetic field service area contained a certain amount of ferromagnetic particle, the character of described cellulose material (hereinafter being also referred to as the output material) was strengthened.
According to the preferred embodiments of the invention, the inventive method comprises following steps: the reactor with reaction volume is provided, fill the described reaction volume of described reactor with multiple material (it participates in physics and/or chemical reaction), the ferromagnetic particle of predetermined proportion is added in the described reaction volume, the reaction volume of described reactor is placed between two inductor blocks at least, so that the magnetic field of described inductor block is interfering with each other in the described reaction volume of described reactor, in the described inductor block each provides the exchange current with predetermined amplitude and frequency.
According to the preferred embodiments of the invention, the mean length of described ferromagnetic particle is in about scope of 0.3 to about 25mm, and preferably in about scope of 3 to about 5mm, diameter is about 0.1 to about 5mm, and preferred about 0.1 to about 2.5mm.Shown that diameter and length ratio are 1: 3 to 1: 5th, especially favourable.According to embodiment preferred, described particle is cylindrical.Based on instruction of the present invention, one skilled in the art will recognize that the size of ferromagnetic particle depends on the input material and can expect optimization according to dropping into, thereby described big I is not in above-mentioned scope.
Can select the size and the shape of ferromagnetic particle according to cellulose Substance Properties, its workability and/or its producibility.Therefore, other size of ferromagnetic particle also can be suitable for the present invention.
Test shows, if when ferromagnetic particle and the ratio that drops into material are about 1 to about 20 weight %, obtains high-quality cellulose material.The content liquid that drops into material is between 0 to about 40%.Yet, in other embodiment of present method, can be according to the workability of cellulose material and/or the particular requirement of producibility are selected other ratios.It depends on the volume of the container of the kind (intermittently or successive) of method and implementation method.In with the embodiment preferred of stem as the input material, the working volume of 2-district container is 180 milliliters, and the quantity of ferromagnetic particle is 14 gram/districts.The particulate mean diameter is 250 microns, and mean length is 1500 microns.Liquid is 1 to 3 with the ratio that drops into material.Container is continuous type.Exposure duration is up to 20 seconds.
Ferromagnetic particle is supported the decomposition of organic materials at ultra-fine born of the same parents and subcellsular level, and born of the same parents are interior and/or the fracture of organic connection of intercellular structure.Compare with the prior art known devices, because the fluidized-bed of the stirring of ferromagnetic particle is applied energy, thereby it has the ability that enhanced destroys the organic materials of all scopes.By machinery crushing, division and/or grinding, up to producing cellulose material more uniformly.The decomposition of organic materials is a key point of the present invention.
Another advantage of the present invention is the mechanical agitation of ferromagnetic particle.Described ferromagnetic particle helps the mixing and the grinding of liquid contents, solvent (if there is) and organic materials, and the quality of cellulose material is further improved.
Described cellulose material has formed the base mateiral of a variety of composite product that are used for multiple shape, form and structure.Described composite prod can or be produced by before-mentioned products is carried out machining subsequently by straight forming method (for example cast, mold, push or extrude).
The service area of electromagnetic field is between the electromagnetic inductor of at least two linearities, and described electromagnetic inductor is separated from each other about 1mm to about 5m, preferred about 50mm gap of about 1m extremely.
The requirement that must satisfy according to described cellulose material and/or described composite article, will drop into material be exposed to electromagnetic field before and/or during,---to be the low-coercivity material---with the ferromagnetic particle of non-memory property be added to drops in the material.
According to production process is step preferred embodiment, and non-ferromagnetic mixing vessel can be exposed in the process of electromagnetic field and serve as container will dropping into material.As requested, described mixing vessel can extend on the whole distance between the inductor block, thereby forms the fluidized-bed that stirs in whole regional space.Other container or the passage that are used for Sequential Production also are suitable for operating the present invention.
In described service area, there is the ferromagnetic particle of non-memory property in the pending input material, promptly the material of low-coercivity is particularly conducive to large-scale operation, and wherein the distance of inductor block is about and is up to 1 meter even several meters.Under the so big situation of the distance between the inductor block, preferably correspondingly increase the quantity of ferromagnetic particle.
The linear electromagnetic inductor block produces the other way around alternating electromagnetic field toward each other.On each point of service area, described inductor block excites the common alternating electromagnetic field, and described electromagnetic field has the circular or oval-shaped hodograph around the magnetic component intensity of the rotation of the common axle between inductor block.The size of magnetic component equals zero on the every bit of described axle, but on each other direction and/or other aspects, magnetic component rises to described inductor block predetermined amplitude.Evidence obtains good result under the following conditions: the amplitude of the center in the 50mm gap between described inductor block is about 0.2 Tesla (SI units: T) to 0.25T, have the 14g ferromagnetic particle in the service area between the inductor block of 180ml container and 50x165x80mm, magnetic force is about 0.03T.The time length that described input material is exposed to described magnetic field is about 20 seconds.
Explain in more detail below described ferromagnetic particle in described service area to described organic materials particulate damaging influence.(B is a magnetic field induction to described ferromagnetic particle by its magnetic component A (A is the vector potential in magnetic field) and B; A is related with B through type B=rotA) in the pair cell and the influence of iuntercellular structure amplify by the decline (causing the magnetic flux increase in this service area) of the magnetic resistance R in the described service area.Term rotA is meant the curl of described vector potential.
Described ferromagnetic particle is at every some H of i place
iIncrease value B under the condition of=constant
iThereby increase the virtual value of gradA.GradA is meant gradient A.
According to the characteristic of the material of described input material and required described cellulose, the magnetic force of the electromagnetic field that is produced by at least two electromagnetic inductors is about 0.01 to about 20T, and preferred about 0.01 arrives about 10T, and most preferably from about 0.03T arrives about 1.2T.
The exposure duration that described input material is exposed to described electromagnetic field is depended on the magnetic force that applies and the material of processing.Be about 1 second to about 3 hours, preferred about 5 seconds to 5 minutes, most preferably from about obtained good result, the material that promptly has the cellulose of good character 20 seconds the time when the time length of described exposure.The degree of uniformity of the material of described cellulose can be regulated by the electrical parameter of described inductor block.
According to embodiment preferred, for the fibrous input material of porphyrize, for example stem carries out the wet grinding step with the high-speed cutting shredder.To be used for dry grinding available from Netzsch-Condux Mahltechnik GmbH, Rodenbacher Chausee 1, D-63457 Hanau/Wolfgang, after the frittering of the CONDUX CS 500 of Germany or CS 1000Z type cut the shredder repacking, be used for carrying out wet grinding to dropping into material at elevated temperatures.
After the wet grinding step, can make intermediate product and---according to other preferred embodiment---mix with other Mierocrystalline celluloses, for example available from Gebr,
Maschinenbau GmbH, Elsener Stra β e 7-9,33102Paderborn, the high-performance Ringlayer Mixer CoriMix of Germany
Mix among the CM.These mixing machines in fact not only mix, and also carry out further homogenizing and pulverizing.Its preferred performance is based on the mixing mechanism of the high circumferential speed that is up to 40m/s.The centrifugal force that causes forms the annular concentric layer of the input material of the liquid contents that comprises at least a organic materials and heat.Annular layer is characterised in that high mixture strength, and it is caused by the high differential between the wall of the mixing tool of the special shape that rotates and mixing machine.Product moves through mixing section with the plug flow form, and the residence time is subjected to the influence of geometrical shape and adjusting and the mixing vessel length and the volumetric flow rate of filling extent, revolution, mixing tool.Mixing section can be divided into zone with different shearing resistances, and preferably with described mixing machine and turbulence mixing machine (be known in and available from
Maschinenbau GmbH) coupling.
In a series of experiments, proved advantageously, with Mierocrystalline cellulose with Microcrystalline Cellulose (MCC)---a kind of high brilliant particle Mierocrystalline cellulose, mainly form by the crystallite aggregation, by hydrolytic deterioration amorphous (cellulosic fibre) zone of the cellulosic raw material of purifying is removed and to obtain---form be added to the cellulose material, the add-on of each batch MCC in each experiment is 5 to 10 weight %, preferred 7 weight %.
The adding of Microcrystalline Cellulose in the time of especially in being added to the input material that mainly contains the cereal stem, generates the cellulose material that is preferably used for producing high strength composite.When the similar mixture of producing with not adding Microcrystalline Cellulose is compared, have the hardness and the tensile strength of increase by the described matrix material of the material production that contains Microcrystalline Cellulose.
Mix after the termination product that described cellulose material promptly can be used for producing matrix material and is used to produce required described cellulose material.
The Technology of the product of production the preferred embodiments of the invention comprises following basic step at least:
1. preparation drops into material (if desired, comprising additive/improving agent) in advance, comprises other above-mentioned production technology;
2. electromagnetism exposes;
3. at least a in curing by described cellulose material and the mold carries out aftertreatment, up to output product (the final article that use).
According to the present invention, step 2 is chosen wantonly.
Term product has contained the finished product (for example panel) and work in-process (for example core material that---such as sandwich structure---is formed by lamination layer structure).Under the latter event, some character of product can be improved, and for example at least one liner is bonded on the described work in-process.The advantage of this class sandwich structure is to give the different character of product (for example structural strength, light structures, resistivity against fire or its combination).According to an embodiment of product, one or several layer or liner available metal, glass or carbon fiber or the preparations of knotting.
According to the present invention, even these anorganic fibers can be added to the input material or be added to the cellulose material after a while.
Perhaps and/or in addition, can carry out suitable surface treatment to the solidified matrix material, it will hereinafter be discussed at this specification sheets.
Drying and/or solidified process are meant the process that excess liq is extracted from the cellulose material.When the moulding of cellulose material,, structure occurs and connect the process of recovering for example by in mould or model, solidifying.This class process is actually n β-glucose molecule residual body and is generally [C to the polymkeric substance formula
6H
7O
2(OH)
3]
nThe integration process of molecular compound.Have 3 oh groups in each residual body [(OH)
3Group] the existence of glucose molecule make between described residual body connection by lateral oh group and therefrom the elimination of water molecule promoted.Therefore, in case the excess liq in the described cellulose material is extracted (for example passing through dehydration or dry under the situation of water), the connection of the structure of organic materials recovers and will take place in the described cellulose material, and causes solidification process.
Be used as at water under the situation of liquid contents, dehydration is undertaken by any known appropriate technology under preset temperature.This class technology comprise and/or combine compression, extrude and filter and absorption, vacuum-drying, air-dry, heating, radiation, beating, under gas blower evaporation and other drying means, for example comprise natural air drying.The selection of concrete grammar of dehydration is depended on process and/or is treated the specific requirement of the article of mold.
According to the characteristic of described fibrous substance and/or treat requirement by the matrix material or the product of its production, the aftertreatment of described cellulose material is by at least a the carrying out in mold, compression mold, the injection mold.Yet other forming technique that is used to produce product also may be suitable.
Undertaken to expect under the situation of aftertreatment that mixing vessel or its part form half of mould simultaneously by compression mold.Because common mold technology is well known by persons skilled in the art, so omit its detailed description.
As requested and workability, carry out mold and curing operation simultaneously or sequentially.
Can carry out other aftertreatment, for example to improve the article made by described matrix material resistance to aqueous vapor or water, or strengthen tolerance, the microbial resistance of described article, or make described matrix material and/or described product have the desired characteristic of resistance, particular color, special smell or its combination based on specific type to the chemical erosion environment.For this purpose, specific properties-correcting agent and/or additive can be joined in the material of described input material and/or described cellulose, and then extract any excessive liquid contents.
As required, described specific properties-correcting agent and/or additive can be used for making the material of described cellulose and/or described matrix material even especially.
Answer special concern following true: the vegetable cell of a few types is coated with or is contained for example inorganic mineral such as silicate or humatite matter oxalate for example of compound.Directly select to contain a certain amount of described compound for example the organic materials of mineral substance can be used for providing the material and the matrix material of cellulose of the present invention, some character that described material and matrix material provide the final user to need.For example, by selecting starting material and adopt described ability, above-mentioned materials can obtain or for example significantly improve below performance characteristic: electroconductibility, thermal conductivity (being heat conductivity), sound insulation, to resistance, chemistry and the microbial exposure etc. of humidity distortion.In addition, if the material of described cellulose does not satisfy the requirement to described matrix material, can add external source properties-correcting agent.
Material with predetermined character (resistance of resistance, wetting ability, the tolerance to the chemical erosion environment, microbial resistance, other and/or specific type, color, smell etc.) is included as the production of the required material of human consumer's hobby by add specific properties-correcting agent in dehydration forward direction uniform substance, and/or in the preparation uniform substance, use special adding technique, be cured and realize.
Now, the simple introduction carried out the some possibilities of surface-treated.According to requirement, can for example obtain some characteristic by for example applying the one layer or more coating by submergence with dipping to the product made by described matrix material.In addition, it is suitable equally to have a coating of particular color.
Method, described matrix material itself that all explanations in the above-mentioned specification sheets all are equally applicable to described cellulose material, produce described matrix material reach the product by its production.
Embodiment 1
The stem portion of selecting cereal is as organic material.Preferably, remove the fringe of described crop.Preferably, after results, obtain stalk.Use wheat stalk in this embodiment.
By the stem that minces stalk stalk being carried out pre-treatment, is about 5-7 millimeter until the mean size of stalk fragment, described fragment is mixed with water and soaks, and the mean diameter of the organic granular in described input material is about 0.8-1mm.In this embodiment, be adjusted to the pH value of aqueous mixture greater than 8.4 and soaked 1.5-2 hour.In other embodiments, soak time was reduced to 1.5-2 minute.1 part of water adds in 3 parts of stalks (w/w).
After immersion, the input material that contains described stalk material is poured into and will be placed two service areas between the inductor block to be used as the stainless steel vessel of mixing vessel.
With the 14g mean diameter is that 250 μ m, mean length are that the cylindrical ferromagnetic particle of 1500 μ m adds in stalk-water mixture in the described container, and the material with described cellulose is exposed to every some H of i place then
iThe electromagnetic field of=constant is worth B with increase
iThereby, the virtual value of increase gradA.
It penetrates (relief width 50mm) 80cm between the inductor block in the described mixing vessel thereby produce alternating electromagnetic field
3Service area.Described magnetic field is provided at that any i point place except that central shaft forms the magnetic component vector of circular and/or oval-shaped hodograph in the space between the described inductor block, thereby makes B
i=μ * H
i, divB wherein
i=0, so rotA
i=B
iThe intensity of described magnetic component equals 0 and the H that satisfies condition at any j point place of described central shaft
j=0, B
j=0 and rotA
j=0.Therefore, the amplitude of generation vector potential A is A in described alternating electromagnetic field
jTo A
iMagnetic field, thereby work in the space of gradA between described inductor block.
Apply the magnetic force of observed value for about 0.3T.Described input material is exposed to described alternating magnetic field 20 seconds.The frequency of described power supply is 50Hz.
When applying described magnetic field, described ferromagnetic particle stirs the input material in the described container tempestuously.In this process, the different i points place in described container, each ferromagnetic particle is all brought into play the effect of mini-sized blender and micropulverizer owing to its interaction with the hodograph of different strength vector H.
After the exposure end of described input material to described electromagnetic field, the organic materials particulate median size that records in the material of staying described cellulose is not less than 1 μ m.Yet the abundant decomposition of described input material has been guaranteed in described magnetic treatment, thereby destructurized with iuntercellular in abundant cell and the cell.
Then, the material of described cellulose is changed over to the mould of B form from mixing vessel.Use suction strainer to increase filtration velocity, thereby then the material of described cellulose is shelved the dry and firm composite material sheet of drying residue.In this embodiment, described evaporative process comprises that the combining method of filtration and seasoning is constant under 30 ℃ temperature until the quality of described matrix material.Carry out structure and strength trial by the control of weight measurement method is dry until described sample.
Embodiment 2 to 13
In the embodiment 3 to 13 of present embodiment 2 and back, used following basic setup.
By the stem that minces stalk wheat stalk being carried out pre-treatment, is about 5-7 millimeter until the mean size of stalk fragment.For the preparation experiment material, the stalk that 100g is minced mixes with the mother liquor of 1000ml.Further make all experiment material precipitations 6 hours before the treatment step.
In experiment 2 to 13, used carboxymethyl cellulose (CMC) separately.The carboxymethyl cellulose (CMC) that is used for these experiments is available from Fischer Chemicals Chemicals AG, and Riesbachstrasse 57, CH-8034Zurich, and Switzerland, CAS number is 9004-32-4.In each experiment, in every kind of experiment material, add 7g CMC and mixing.Other the experiment in used Microcrystalline Cellulose (MCC), according to its mean size of embodiment preferred between about 15 to 40 microns.
Among four of described experiment, material is exposed to the aforesaid electromagnetic field that produces between linear electromagnetic inductor service area will be dropped into.The time that is exposed to electromagnetic field is listed in " inductor block " row of following table 1.
In experiment 3,6,9 and 12, with the stalk material boiling in the mother liquor 3 hours, shown in " boiling " in following table row.The mixture based on NaOH of embodiment 12 is neutralized after boiling.
Then all laboratory samples are all transferred on the filter paper.Push and remove excessive water, make remaining filter cake precipitation 2 hours then.
Experiment 2,5,8 and 11 sample is exposed in the service area between the inductor block 1 minute, then it is transferred to strainer.
In 80 to 85 ℃ temperature is with dry 16 or 24 hours of all samples, shown in " drying " row afterwards.
Table 1: experiment 2 to 13
Disclosed according to the material of embodiment 2 and 5 preparations the hardest and the firmest to testing the nonstandardized technique mechanical test that the gained coupon carries out in 2 to 13.All samples according to experiment 2 to 8 and 11 to 13 preparations shows that the cellulose material is suitable for the mixture of production moulding.Yet, use inherent strength and stability to be considered to lower according to the coupon of the cellulose material production of embodiment 9 and 10.
Embodiment 14
By the stem that minces stalk wheat stalk being carried out pre-treatment, is about 5-7 millimeter until the mean size of stalk fragment.For the preparation experiment material, the stalk that 100g is minced mixes with 1000ml hot water.All experiment materials carry out wet grinding immediately in CONDUX Fine cutting mills CS 500 (available from Netzsch-Condux) after making.In the wet grinding process, the temperature range of the mixture of water and stalk preferably is maintained at about 92 to 94 ℃.The product that grinds is very thin and even, has been fit to produce matrix material and has produced the required product that contains described cellulose material.
Embodiment 15
By the stem that minces stalk wheat stalk being carried out pre-treatment, is about 5-7 millimeter until the mean size of stalk fragment.For the preparation experiment material, the stalk that 100kg is minced mixes with 1000l hot water.All experiment materials carry out wet grinding immediately in CONDUX Fine cutting mills CS 500 (available from Netzsch-Condux) after making.In the wet grinding process, the temperature range of the mixture of water and stalk preferably is maintained at about 92 to 94 ℃.In the wet grinding process, aqueous, liquid cellulose is partly separated and is discharged from mill.In capable of circulation time mill of the liquid portion of described heat.Yet according to embodiment preferred, this hot liquid portion further concentrates by filtration or dehydration and adds in mixing process.Again at high-performance Ringlayer Mixer CoriMix available from Gebr.Lodige Maschinenbau GmbH
Mix among the CM.
Above-mentioned experiment shows, according to the present invention, has strengthened the character of prepared material and material based on the adding of cellulosic tackiness agent and binding agent (preferably with water-soluble form, as methylcellulose gum and Walocel MT 20.000PV).In other embodiment preferred, add Microcrystalline Cellulose and/or powdery cellulose to reach other required character.
Claims (26)
1. method of producing the cellulose material, described method comprises following steps:
Preparation comprises the input material of at least a organic materials and a kind of liquid contents; With
With described input expect in 70 to 120 ℃, preferred 80 to 100 ℃, most preferably the temperature in 92 to 94 ℃ of scopes is carried out wet mixing.
2. the method for claim 1 is included in the wet mixing process or separates the step of aqueous, liquid cellulose part afterwards.
3. claim 1 or 2 method comprise and add other Mierocrystalline celluloses in described cellulose materials, the step of preferable methyl Mierocrystalline cellulose and/or carboxymethyl cellulose---preferably with sodium-salt form---and/or Microcrystalline Cellulose,
Perhaps after concentrated or dehydration, return and add cellulosic step by the cellulose part that will produce in the wet mixing step.
4. the method for one of aforementioned claim wherein described input material is exposed to the service area of electromagnetic field, and described input material preferably comprises a plurality of ferromagnetic particles.
5. the method for claim 4, the mean length of wherein said ferromagnetic particle is in about scope of 0.3 to about 25mm, preferably in about scope of 3 to about 5mm; And the mean diameter of wherein said ferromagnetic particle is in about scope of 0.1 to about 5mm, preferably in about scope of 0.1 to about 2.5mm.
6. claim 4 or 5 method, the diameter of wherein said ferromagnetic particle is about 1: 3 to 1: 5 with the ratio of length, and preferably is cylindrical haply.
7. the method for one of claim 4 to 6, the ratio of wherein said ferromagnetic particle and described input material are about 1 to about 25 weight %, preferred about 10 to 15 weight %.
8. the method for one of claim 2 to 7, wherein said service area results between the linear electromagnetic inductor block, described electromagnetic inductor produces from opposite direction electromagnetic field toward each other, wherein said inductor block preferably excites the common alternating electromagnetic field, and described electromagnetic field has the circular or oval-shaped hodograph around the magnetic component intensity of the rotation of the common axle between described inductor block.
9. the method for claim 8, wherein said electromagnetic inductor are separated from each other 1mm to about 5m, preferred about 50mm distance of about 1m extremely.
10. claim 8 or 9 method, the magnetic force of wherein said electromagnetic inductor are about 0.01 to about 20 teslas, and preferred about 0.01 to about 10 teslas.
11. the method for one of claim 2 to 10, the time length of wherein said exposure is about 1 second to about 3 hours, preferred about 5 seconds to about 5 minutes, and most preferably from about 20 or 60 seconds.
12. the method for claim 11, wherein said organic materials comprises fiber.
13. the method for claim 11 or 12, wherein said organic materials is derived from higher plant, preferably is selected from very grass of Gramineae (Poaceae) class, preferred especially cereal crop; Cotton; Hemp; Flax or its mixture.
14. the method for claim 13, wherein said organic materials are derived from least a in grain stem and the rice straw.
15. the method for one of claim 2 to 14, wherein said liquid contents comprise at least a in water and the solvent.
16. the method for one of claim 2 to 15, wherein said organic materials by be about 8 in the pH value, more preferably greater than 8, most preferably greater than 8.4 liquid in dipping, dynamo-electric effect, fluid power effect, ultrasonic wave effect, boil, at least a in the decatize carries out pre-treatment.
17. a cellulose material is made by the method for one of claim 1 to 16.
18. produce the method for the matrix material of the cellulose material that comprises claim 17.
19. the method for claim 18 wherein is added at least a additive or properties-correcting agent at least a in described input material or the described cellulose material.
20. the method for claim 18 or 19 is wherein with described cellulose material homogenizing.
21. the method for one of claim 18 to 20, wherein said cellulose material carries out aftertreatment through at least a in mold, compression mold, the injection mold.
22. the method for claim 21, the excessive part of wherein said liquid contents is by at least a extraction the in dry or the curing.
23. a matrix material is made by the method for one of claim 17 to 22.
24. a product is made by the matrix material of claim 23.
25. the product of claim 24 by dipping, for example is coated with by immersion.
26. the product of claim 24 or 25 comprises at least one liner, it is bonded in through on the cellulose material of aftertreatment.
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| CH01532/09A CH701959B1 (en) | 2009-10-01 | 2009-10-01 | Cellulosic mass. |
| PCT/EP2010/064189 WO2011039121A1 (en) | 2009-10-01 | 2010-09-24 | Cellulose-containing mass |
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| US (1) | US20120193048A1 (en) |
| EP (1) | EP2483345A1 (en) |
| JP (1) | JP2013506723A (en) |
| CN (1) | CN102159637A (en) |
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| CH (1) | CH701959B1 (en) |
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| CH704766A1 (en) * | 2011-04-01 | 2012-10-15 | Vadim Gogichev | A process for preparing a cellulose-containing material for producing a composite material. |
| CN113182023B (en) * | 2021-04-21 | 2022-06-03 | 南京工程学院 | On-line detection method for mill load of non-measurable disturbance self-adaptive monitoring and compensation |
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| CN101062572A (en) * | 2006-04-29 | 2007-10-31 | 山东贺友集团有限公司 | New technique for producing wood-plastic clad plate |
| CN101099070A (en) * | 2004-11-12 | 2008-01-02 | 密歇根生物技术研究所 | Process for treatment of biomass feedstocks |
| WO2010064069A1 (en) * | 2008-12-03 | 2010-06-10 | Vadim Gogichev | Cellulose-containing mass |
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| GB592633A (en) * | 1945-04-25 | 1947-09-24 | English Metal Powder Company L | Metal-containing cellulose-acetate films |
| US3691130A (en) * | 1970-08-06 | 1972-09-12 | Dmitry Danilovich Logvinenko | Method of producing metal-polymer compositions |
| US4093189A (en) * | 1976-10-18 | 1978-06-06 | Iosif Borisovich Sokol | Apparatus for continuous preparation of a suspension |
| FR2378084A1 (en) * | 1977-01-21 | 1978-08-18 | Rostovsky O Neftemaslozavod | PROCESS FOR PREPARING PLASTIC AND LIQUID LUBRICANTS |
| US4601431A (en) * | 1982-09-13 | 1986-07-22 | Fuji Electric Company, Ltd. | Traveling magnetic field type crusher |
| US5139861A (en) * | 1990-06-21 | 1992-08-18 | E. I. Du Pont De Nemours And Company | Process for bonding blends of cellulosic pulp and fusible synthetic pulp or fiber by high-speed dielectric heating and products produced thereby |
| EP1220031A3 (en) * | 2000-12-29 | 2002-08-14 | Eastman Kodak Company | Film support with improved adhesion upon annealing |
| GB0101630D0 (en) * | 2001-01-23 | 2001-03-07 | Amylum Europ Nv | Method for preparing composite materials containing natural binders |
| WO2004000446A2 (en) * | 2002-06-20 | 2003-12-31 | Arizona Board Of Regents | Method and arrangement of rotating magnetically inducible particles |
| US7576147B2 (en) | 2004-08-27 | 2009-08-18 | Board Of Trustees Of Michigan State University | Cellulosic biomass soy flour based biocomposites and process for manufacturing thereof |
| EP2415807A3 (en) * | 2006-10-26 | 2012-10-31 | Xyleco, Inc. | Method of making butanol from biomass |
| US7579396B2 (en) | 2007-01-31 | 2009-08-25 | Eastman Kodak Company | Polymer composite |
| CH700073A2 (en) * | 2008-12-03 | 2010-06-15 | Corp Vadim Gogichev C O Kremlin Group | Current generator, e.g. galvanic cell for supplying medicinal implants, comprises separating layer containing zwitterionic and/or radical compound between two electrodes |
| FR2940297B1 (en) * | 2008-12-18 | 2013-12-20 | Ab7 Ind | COMPOSITE PLASTIC MATERIAL IN THE FORM OF GRANULATES FROM PLANT PROTEIN MATERIALS AND METHOD OF MANUFACTURING THE SAME |
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2009
- 2009-10-01 CH CH01532/09A patent/CH701959B1/en not_active IP Right Cessation
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2010
- 2010-09-24 JP JP2012531336A patent/JP2013506723A/en not_active Withdrawn
- 2010-09-24 CA CA2774506A patent/CA2774506A1/en not_active Abandoned
- 2010-09-24 US US13/498,870 patent/US20120193048A1/en not_active Abandoned
- 2010-09-24 CN CN2010800034722A patent/CN102159637A/en active Pending
- 2010-09-24 EP EP10757768A patent/EP2483345A1/en not_active Withdrawn
- 2010-09-24 MX MX2012003895A patent/MX2012003895A/en not_active Application Discontinuation
- 2010-09-24 EA EA201270501A patent/EA201270501A1/en unknown
- 2010-09-24 WO PCT/EP2010/064189 patent/WO2011039121A1/en active Application Filing
- 2010-09-24 BR BR112012007295A patent/BR112012007295A2/en not_active Application Discontinuation
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101099070A (en) * | 2004-11-12 | 2008-01-02 | 密歇根生物技术研究所 | Process for treatment of biomass feedstocks |
| CN101062572A (en) * | 2006-04-29 | 2007-10-31 | 山东贺友集团有限公司 | New technique for producing wood-plastic clad plate |
| WO2010064069A1 (en) * | 2008-12-03 | 2010-06-10 | Vadim Gogichev | Cellulose-containing mass |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109705600A (en) * | 2018-12-28 | 2019-05-03 | 广州鸿绵合成材料有限公司 | A kind of high-performance ligno cellulose fiber and preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CH701959A1 (en) | 2011-04-15 |
| WO2011039121A1 (en) | 2011-04-07 |
| CA2774506A1 (en) | 2011-04-07 |
| JP2013506723A (en) | 2013-02-28 |
| US20120193048A1 (en) | 2012-08-02 |
| EP2483345A1 (en) | 2012-08-08 |
| MX2012003895A (en) | 2012-07-25 |
| BR112012007295A2 (en) | 2016-04-19 |
| EA201270501A1 (en) | 2012-09-28 |
| CH701959B1 (en) | 2012-04-30 |
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