CN103924471B - A kind of preparation of modified wood fibre element and its product - Google Patents
A kind of preparation of modified wood fibre element and its product Download PDFInfo
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- CN103924471B CN103924471B CN201410139457.0A CN201410139457A CN103924471B CN 103924471 B CN103924471 B CN 103924471B CN 201410139457 A CN201410139457 A CN 201410139457A CN 103924471 B CN103924471 B CN 103924471B
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Abstract
The invention discloses a kind of preparation method of modified wood fibre element, including 1), by lignocellulosic material precrushing；2), the lignocellulosic material of precrushing is pre-processed；3), reactor is preheated, the pH value added in pretreated feedstock, control reactor is subsequently passed saturated vapor, reaction maintains a period of time under certain temperature and pressure；4) after, reaction terminates, stop logical steam, be subsequently passed condensed water, until reactor is cooled to normal temperature；5), reactant is then ground to certain particle size by washing, filtering, dry.Modified wood fibre element prepared by this method has hydrophobic and resistant to elevated temperatures characteristic, can be particularly suitable for use in engineering plastics as plastic filler.
Description
Technical field
The present invention relates to a kind of preparation method of modified wood fibre element and its product.The wooden fibre of modification prepared by this method
Dimension has hydrophobic and resistant to elevated temperatures feature, can be particularly suitable for use in engineering plastics as plastic filler.
Background technology
Lignocellulose biomass exists in the form of plant, and main component is cellulose, hemicellulose and lignin.
The annual lignocellulose biomass total amount generated by photosynthesis is more than 200,000,000,000 tons on the earth, therefore lignocellulosic biomass
Matter is renewable resource most abundant, most cheap on the earth.
The easy moisture absorption of thermoplastic composite, the easily expansion prepared using lignocellulosic as filler.Although expansion can lead to
Addition coupling agent is crossed to suppress, but in a humidity environment, material can still be expanded over time.If in addition,
Bacteriostatic agent or insecticide are not added in process of production, and wood plastic composite is easy in soil or under moist environment
By microbiologic(al) corrosion.In addition in the process of Wood-plastic material, if heat treatment degree is excessively fierce, lignocellulosic is easily sent out
Raw degraded produces smell.When being heated to 160 DEG C such as timber, ether bond rupture generation oligosaccharide and list will occur for hemicellulose
Sugar.Therefore, the type of polymer that lignocellulosic can be applicable as filler is less.
Research finds that material can be made up to 300 except hemicellulose by largely reducing or removing in primary lignocellulosic
DEG C when extrusion or injection molding process in will not produce gas, while hemicellulose go decapacitation so that material hydrophily be deteriorated
(because content of lignin hydrophobic in material is improved).
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of preparation method of modified wood fibre element.Pass through the party
Modified wood fibre element prepared by method has hydrophobic and resistant to elevated temperatures characteristic, can be particularly suitable for use in engineering as plastic filler
Plastics.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation of modified wood fibre element, comprises the following steps：
1), by lignocellulosic material precrushing；
2), the lignocellulosic material of precrushing is pre-processed；
3), reactor is preheated, the pH value added in pretreated feedstock, control reactor is subsequently passed saturated vapor, instead
A period of time should be maintained under certain temperature and pressure；
4) after, reaction terminates, stop logical steam, be subsequently passed condensed water, until reactor is cooled to normal temperature；
5), reactant is then ground to certain particle size by washing, filtering, dry.
Prepared modified wood fibre element has hydrophobic and resistant to elevated temperatures characteristic, can especially be fitted as plastic filler
For engineering plastics.
Preferably, described lignocellulosic material refers to any kind of plant biomass, such as, but not limited to, non-
Xylophyta biomass, imtertilled crop, such as, but not limited to, straw or like vegetable, such as, but not limited to, switchgrass, Value of Spartina Anglica, black
Wheat straw, Chinese silvergrass, reed canary grass or its combination；The residue of carbohydrate processing, such as, but not limited to, bagasse, beet pulp or its combination；Agriculture
Crop material, such as, but not limited to, paddy, wheat, corn, beans, potato class, oil plant, cotton or its combination；Forestry biomass
Matter, such as, but not limited to, firewood forests, the scattered timber in the tending of woods and Chose cutting, the branch of residual, leaf, wood
Bits or its combination；Forest trimmings, such as, but not limited to, branch, sawdust, wood shavings, the tip of a branch in logging and process,
Slab, butt or its combination；The discarded object of forestry byproductses, such as, but not limited to, shell, fruit stone or its combination.In addition,
The lignocellulosic material may include Paper or cardboard dead meal, such as, but not limited to old and useless newspaper and cardboard etc..Wood fibre
Plain raw material may include a type of fiber, also may include to come from the former various fibre blends of different lignocellulosics.In addition,
The lignocellulosic material may include fresh lignocellulosic material, the lignocellulosic material of local desiccation, fully do
Dry lignocellulosic material or its combination.In addition, any of the above described species can be made new by plant breeding or genetic engineering
Lignocellulosic material.
Preferably, the content of cellulose of the lignocellulosic material is approximately more than 20%, and more preferably approximately more than 30%,
Still more preferably it is approximately more than 40%.In addition, the content of lignin of the lignocellulosic material is approximately more than 10%, more allusion quotation
Type is approximately more than 15%.The lignocellulosic material also may include a small amount of sucrose, fruit sugar and starch.
Preferably, the precrushing method of the lignocellulosic material include but is not limited to mill, grind, stir, powder
Broken, compression/expansion or other types of mechanically actuated.Crushed, can be set using any kind of be applicable by mechanically actuated
It is standby, such as, but not limited to beater grinder, drum-type crusher, roll press, refiner, mixer grinder, ball mill and vertical
Formula grinding machine.By above-mentioned break process, the length of at least 80% raw material is changed into below 1cm, preferably at least 90% raw material
Length is changed into below 5mm.
Preferably, the preprocess method of the lignocellulosic material is preimpregnation.The pre-preg reagent be alkali lye,
Water and dilute acid soln.
Preferably, the alkali lye has NaOH, Na2CO3、NaHCO3、Na2SO3Or its composition；The pickle carrys out bin cure
Acid, hydrochloric acid, nitric acid, phosphoric acid or its composition.The concentration of the alkali lye or pickle is 0.05~2.5M, preferably 0.1~1.5M.
The preimpregnation time is 10~180min, preferably 30~120min；The preimpregnation temperature is 40~120 DEG C, preferably 60~100
℃；The mass ratio of the prepreg solution and the lignocellulosic material is 1: 5~40, preferably 1: 5~20.
Preferably, the pH value in the reactor is controlled below 7, and preferably 4~6.5；The reaction pressure of the reactor
Power is in 0.5~5MPa, preferably 1~2MPa；Reaction temperature in the reactor is at 150~250 DEG C, preferably 180~220 DEG C；
The reaction time maintains 2~12h, preferably 4~8h.
Preferably, the reactant is washed with deionized to filtrate in neutrality, is dried at 80~120 DEG C to aqueous
Amount is below 10%.
Preferably, the dried product exhibited further crush and sieve.Breaking method includes but is not limited to mill,
Grinding, agitation, crushing, compression/expansion or other types of mechanically actuated.Crushed, can be used any by mechanically actuated
The suitable device of type, such as, but not limited to beater grinder, drum-type crusher, roll press, refiner, agitation grinding
Machine, ball mill and vertical grinder.
Preferably, the equipment that the precrushing of the lignocellulosic material is further crushed with dried product exhibited is respective
Independent equipment, can be identical, also can be different.
Preferably, the modified wood fibre element is at 30 DEG C, and relative humidity is placement in 90% climatic chamber
24h, its water absorption rate is less than 10%, preferably smaller than 5%.
Preferably, the decomposition temperature of the modified wood fibre element is more than 290 DEG C.
Brief description of the drawings
Fig. 1 is the differential heat determination curve of thermogravimetric one of modified wood fibre.
Fig. 2 is the plain water absorption rate comparison diagram with untreated lignocellulosic of modified wood fibre.
Embodiment
Embodiment 1
10kg wood shavings ball mill precomminution is taken to 20 mesh sieves excessively；Add concentration be 0.5M hydrochloric acid solution, make wood shavings with
The solid-to-liquid ratio of hydrochloric acid solution reaches 1: 10, and hot submersion groove maintains 60min to 80 DEG C；Reactor is preheated to 150 DEG C, plus
Enter and impregnate thing, the pH value in control retort is subsequently passed saturated vapor to reacting kettle inner pressure and reached 5.5 or so
1.5MPa, and reactor temperature is controlled in 220 DEG C, sustained response 5.5h；After reaction terminates, stop logical steam, be subsequently passed
Condensed water to reactor is cooled to normal temperature；Reactant passes through with pure water to filtrate in neutral, is dried overnight at 80 DEG C, then
2h is dried at 105 DEG C to product moisture content less than 10%；Finally with grinder grinding product to 100 mesh sieves excessively.
Take modified lignocellulosic example weight 10mg with thermogravimetric-differential heat while determining decomposition temperature, it determines bar
Part is measure under nitrogen atmosphere, and programming rate is 10 DEG C per minute, and reference sample is alpha-aluminium oxide.Test result such as Fig. 1 institutes
Show, decomposition temperature TDThe intersection point D of the tangent line of start temperature and the tangent line of weight reduction end temp is reduced for the weight of TG curves
Temperature.Calculate decomposition temperature TDFor 311 DEG C.
By the plain and unmodified lignocellulosic of modified wood fibre at 30 DEG C, relative humidity is 90% constant temperature and humidity
24h, calculating water absorption rate of then weighing are placed in case.Test result is as shown in Fig. 2 the water absorption rate of modified lignocellulosic is
4.85%, unmodified sample water absorption rate is 36.82%.This is due to the easy decomposition in lignocellulosic at reaction conditions
Composition -- hemicellulose is decomposed first, and hemicellulose can absorb water.Hemicellulose level is reduced, modified lignocellulosic
Water absorption rate declines.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details.
Claims (12)
1. a kind of preparation method of modified wood fibre element, comprises the following steps：
1）, by lignocellulosic material precrushing；
2）, precrushing lignocellulosic material pre-processed；
3）, reactor preheated, the pH value added in pretreated feedstock, control reactor is subsequently passed saturated vapor, reaction exists
A period of time is maintained under certain temperature and pressure；
4）, after reaction terminates, stop logical steam, be subsequently passed condensed water, until reactor is cooled to normal temperature；
5）, reactant by washing, filtering, dry, be then ground to certain particle size；
Prepared modified wood fibre element has hydrophobic and resistant to elevated temperatures characteristic, can be filled out as general-purpose plastics and engineering plastics
Material.
2. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：Described wooden fibre
The plain raw material of dimension includes residue, agricultural crop straw, forestry biomass, forest trimmings, forestry byproductses that straw or like vegetable, carbohydrate are processed
Discarded object；In addition, the lignocellulosic material may include Paper or cardboard dead meal；Lignocellulosic material may include one kind
The fiber of type, also may include to come from the former various fibre blends of different lignocellulosics；In addition, the lignocellulosic is former
Material may include that fresh lignocellulosic material, the lignocellulosic material of local desiccation, fully dry lignocellulosic are former
Material or its combination；In addition, lignocellulosic material can be made by plant breeding or genetic engineering in any of the above described species.
3. a kind of preparation method of modified wood fibre element according to claim 1 or 2, it is characterised in that：It is described wooden
The content of cellulose of cellulosic material is more than 20%；The content of lignin of the lignocellulosic material is more than 10%；It is described wooden
Cellulosic material also may include a small amount of sucrose, fruit sugar and starch.
4. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：The wood fibre
The precrushing method of plain raw material includes milling, grinding, stirring, crushing or compression/expansion；Beater grinder, cartridge type powder can be used
Broken machine, roll press, refiner, mixer grinder, ball mill or vertical grinder carry out precrushing；By above-mentioned broken place
Reason, the length of at least 90% raw material is changed into below 5mm.
5. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：The wood fibre
The preprocess method of plain raw material is preimpregnation；The pre-preg reagent is alkali lye, water and dilute acid soln.
6. a kind of preparation method of modified wood fibre element according to claim 5, it is characterised in that：The alkali lye has
NaOH、Na2CO3、NaHCO3、Na2SO3Or its composition；The dilute acid soln comes from sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or its combination
Thing；The concentration of the alkali lye or dilute acid soln is 0.05~2.5M；The preimpregnation time is 10~180min；The preimpregnation temperature
For 40~120 DEG C；The mass ratio of the prepreg solution and the lignocellulosic material is 1:5~40.
7. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：In the reactor
PH value control 4~6.5；The reaction pressure of the reactor is in 0.5~5MPa；Reaction temperature in the reactor exists
150~250 DEG C；The reaction time maintains 2~12h.
8. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：The reactant is used
Deionized water is washed to filtrate in neutrality, is dried at 80~120 DEG C to water content below 10%.
9. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：Produced after the drying
Thing further crush and sieve；Breaking method includes milling, grinding, stirring, crushing or compression/expansion；Hammer can be used
Pulverizer, drum-type crusher, roll press, refiner, mixer grinder, ball mill or vertical grinder are crushed.
10. a kind of preparation method of modified wood fibre element according to claim 1 or 4 or 9, it is characterised in that：It is described
The precrushing of lignocellulosic material is each independent equipment with the equipment that dried product exhibited is further crushed, can be identical, also
Can be different.
11. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：Pass through the system
The modified wood fibre element of Preparation Method production is at 30 DEG C, and relative humidity is places 24h in 90% climatic chamber, and it absorbs water
Rate is less than 10%.
12. a kind of preparation method of modified wood fibre element according to claim 1, it is characterised in that：Pass through the system
The decomposition temperature of the modified wood fibre element of Preparation Method production is more than 290 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112397850A (en) * | 2020-11-12 | 2021-02-23 | 同济大学 | Modified lignocellulose diaphragm for lithium ion battery and preparation method and application thereof |
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| CN105457606A (en) * | 2015-12-11 | 2016-04-06 | 上海同化新材料科技有限公司 | Filter aid for metal calendering and rolling oil |
| CN106117463A (en) * | 2016-06-26 | 2016-11-16 | 吴迪 | A kind of biodegradable oil absorption process for preparing resins |
| CN106084852A (en) * | 2016-08-05 | 2016-11-09 | 宁波金特信钢铁科技有限公司 | A kind of preparation method of automobile-used biological engineering plastics |
| CN109728315A (en) * | 2018-12-27 | 2019-05-07 | 华北电力大学 | Modified carbonized celulose cardboard electrode material and microbiological fuel cell |
| CN110628844A (en) * | 2019-09-23 | 2019-12-31 | 福建生物工程职业技术学院 | Graded separation method for cord grass |
| CN110774397A (en) * | 2019-11-22 | 2020-02-11 | 上海同化新材料科技有限公司 | Production system and production method of bleached lignocellulose |
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| CN1141373A (en) * | 1995-07-22 | 1997-01-29 | 池洪 | Plant fiber material and preparation process thereof |
| CN1563564A (en) * | 2004-03-16 | 2005-01-12 | 山东轻工业学院 | Method for producing chemical wood pulp |
| CN101068977A (en) * | 2004-10-04 | 2007-11-07 | 梅特索纸业股份有限公司 | Alkaline process and system for producing pulp |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141373A (en) * | 1995-07-22 | 1997-01-29 | 池洪 | Plant fiber material and preparation process thereof |
| CN1563564A (en) * | 2004-03-16 | 2005-01-12 | 山东轻工业学院 | Method for producing chemical wood pulp |
| CN101068977A (en) * | 2004-10-04 | 2007-11-07 | 梅特索纸业股份有限公司 | Alkaline process and system for producing pulp |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112397850A (en) * | 2020-11-12 | 2021-02-23 | 同济大学 | Modified lignocellulose diaphragm for lithium ion battery and preparation method and application thereof |
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