CN107476104B - A kind of preparation method with hydrophobic wood fibre and its product - Google Patents
A kind of preparation method with hydrophobic wood fibre and its product Download PDFInfo
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- CN107476104B CN107476104B CN201710683879.8A CN201710683879A CN107476104B CN 107476104 B CN107476104 B CN 107476104B CN 201710683879 A CN201710683879 A CN 201710683879A CN 107476104 B CN107476104 B CN 107476104B
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- preparation
- wood fibre
- hydrophobic
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- lignocellulose
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
-
- 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
- D21C1/00—Pretreatment of the finely-divided materials before digesting
- D21C1/04—Pretreatment of the finely-divided materials before digesting with acid reacting compounds
Abstract
The present invention provides a kind of preparation methods with hydrophobic wood fibre, the preparation method is that lignocellulose raw material drying sieving is first obtained lignocellulose, acidolysis is carried out to lignocellulose at 80-120 DEG C using the concentrated sulfuric acid, the acidolysis time is 60-120 minutes, alkalization and degreasing are carried out to material at 120-160 DEG C with lye and rosin again, alkalization and degreasing time are 180-240 minutes, then material is down to room temperature, filter out mother liquor, the pH value of material is adjusted between 6-8 with diluted acid, material is followed by stirring and washing at 50-70 DEG C, it is washed again with the hot water added with siloxanes, finally material is put into 110 DEG C of drier and is dried, up to product.Preparation method of the invention, operating condition is simple, safe, and the reaction time is short, and washing is easy, and the good product dispersibility of acquisition, effect of prestressed is good, intensity is high, hydrophobic effect greatly improves.Has the function of hydrophobic wood fibre by what above-mentioned preparation method obtained the present invention also provides a kind of, the wood fibre is particularly suitable for being added in concrete mortar or plastering.
Description
Technical field
The present invention relates to a kind of preparation method of wood fibre more particularly to a kind of waste wood, woodenware leftover bits and pieces, sawdust,
The preparation method of the natural wooden fibers such as bagasse, cotton linter, crudefiber crop, specifically relating to one kind has the function of the wooden fibre of hydrophobic
The preparation method of dimension.The invention further relates to a kind of wood fibres obtained by above-mentioned preparation method.
Background technique
Wood fibre is that the organic cotton-shaped or powdery that natural reproducible timber is processed by chemical treatment, Mechanical Method is fine
Tie up substance, can be widely used for the fields such as concrete mortar, plastering, wood pulp sponge, asphalt roads, to prevent coating cracking,
Raising water-retaining property, the conformance for improving the stability and construction that produce, increase intensity, enhancing have well the adhesive force on surface etc.
Effect.In addition, the moisture of internal system can be transmitted rapidly since wood fibre has the capillarity of fibre structure
To pulp surface and interface, so that the uniform moisture inside slurry is distributed, skinning can obviously reduce, and make bonding strong
Degree and surface strength significantly improve, this mechanism is but also mortar is obviously played anti-due to the reduction of tension in the drying process
The effect split, while the dimensional stability of wood fibre and thermal stability also play good thermal-insulating and anti-cracking in thermal insulation material
Effect.But it joined the later mortar of wood fibre, water absorption increases, and water-fast, weatherability reduces, and therefore, has researched and developed one kind both
It is able to maintain the existing characteristic of wood fibre, again with the novel wooden fiber of certain hydrophobic function, is those skilled in the art's cause
The project of power research.
Summary of the invention
To solve the problems, such as present on, the object of the present invention is to provide a kind of preparations with hydrophobic wood fibre
Method, this method is simple, safe operation.
It is a further object of the present invention to provide a kind of products obtained by above-mentioned preparation method.
In order to achieve the above object, the preparation method with hydrophobic wood fibre of the invention, primary includes following step
It is rapid:
(1) lignocellulose raw material to be dried, crush, cross 60 meshes, drying to constant weight at 60-130 DEG C for screenings, after
70 meshes, obtain lignocellulose；
(2) lignocellulose and water are put into reactor for 1:4-6 in mass ratio, are gradually added wood after mixing evenly
The concentrated sulfuric acid of matter cellulose powder amount 2-5% is acidified, and enriching sulfuric acid process is stirred continuously, and cellulose powder is prevented to be carbonized, and will be reacted
Device is heated to 80-120 DEG C and is stirred continuously, and moisture evaporation situation adds a certain amount of water in whipping process visual response device, to protect
Material energy uniform stirring is held, stops adding water after 60-120 minutes, continues stirring to material in paste-like, stops heating；
(3) lye for being slowly added to 4-7 times of lignocellulose amount alkalizes, stirring while adding, measures the pH of material
When value is greater than 8, the rosin that 0.2-1 times of lignocellulose amount is added carries out degreasing, continues to be heated to 120-160 DEG C, react
The appropriate water supplement of slurry consistency is regarded in journey, to keep material energy uniform stirring, is reacted 180-240 minutes, is stopped heating；
(4) material is down to room temperature, filters out mother liquor, the pH value of dilute acid soln adjusting material is added between 6-8, heating
It is warming up to 50-70 DEG C material is followed by stirring and washing, wash time is greater than 30 minutes, then is carried out with the hot water added with siloxanes
Washing, the mass concentration of siloxanes aqueous solution are 5%-10%, and hot water temperature controls at 40-70 DEG C；
(5) it will be put into 110 DEG C of drier and dried to get the wood fibre with hydrophobic function after material filtering.
In above-mentioned preparation method, the lignocellulose raw material of step (1) be waste wood, weedtree, woodenware processing factory leftover bits and pieces
Or sawdust.
In order to keep the mixing of siloxanes and wood fibre more uniform, the more preferable hydrophobicity for improving wood fibre, above-mentioned system
In Preparation Method, for the number for using siloxanes hot water to wash in step (4) for 2-5 times, the dosage of each siloxanes hot water is 500-
1000ml, total wash time are greater than 30 minutes.
It is required to make product reach certain whiteness, in above-mentioned preparation method, step (4) carries out siloxanes heat to material
Before water washing, sodium hypochlorite is first added and carries out bleaching, the additional amount of sodium hypochlorite is effective chlorine in material in 0.05-
Between 0.1g/100g.
In above-mentioned preparation method, the concentrated sulfuric acid of step (2) is the concentrated sulfuric acid that commercial available quality concentration is 98%.
In above-mentioned preparation method, the lye of step (3) is to be dissolved to be formed by solid sodium hydroxide or potassium hydroxide, lye matter
Amount concentration is 20%-56%.
In above-mentioned preparation method, the diluted acid of step (4) is the dilute sulfuric acid that mass concentration is 2%-5%.
Has the function of hydrophobic wood fibre by what above-mentioned preparation method obtained the present invention also provides a kind of.
The preparation method with hydrophobic wood fibre of the invention first carries out lignocellulose using the concentrated sulfuric acid
Acidolysis softens the capillary of lignocellulose sufficiently, then carries out alkalization and degreasing with lye and rosin, and rosin is anti-with alkali
The rosin soap that should be formed can remove the impurity of wood fibre very well, guarantee the purity of wood fibre, finally with added with siloxanes
Hot water washed, so that siloxane polymer is sufficiently adsorbed on the capillary surface of lignocellulose, reach good
Hydrophobic effect.Preparation method of the invention, operating condition is simple, safe, and the reaction time is short, and washing is easy, the product point of acquisition
Scattered property is good, effect of prestressed is good, intensity is high, hydrophobic effect greatly improves, particularly suitable for being added to concrete mortar or gypsum system
In product.
Detailed description of the invention
Fig. 1 is the gypsum product cracking situation for adding commercially available wood fibre.
Fig. 2 is the gypsum product cracking situation for adding wood fibre of the present invention.
Specific embodiment
Here is that have the function of several embodiments of hydrophobic wood fibre by raw material preparation of sawdust, but these embodiments are only
It is to be illustrated to technical solution of the present invention, the protection scope being not intended to limit the invention is not departing from theory of the present invention
Under the premise of, change or replacement to raw material sources are within the scope of protection of the invention.
One, embodiment
Embodiment 1
By sawdust drying, it crushed 60 meshes, drying to constant weight at 70 DEG C for screenings continuation, after 70 meshes, takes sieve
Lower wood dust 100g is put into reactor, and 400g water is added, and is gradually added the sulfuric acid acid that 2g mass concentration is 98% after mixing evenly
Change, adds sulfuric acid process needs to be stirred continuously, prevent cellulose powder to be carbonized, measure its pH value between 1-5, reactor is heated to
80 DEG C, and be stirred continuously, moisture evaporation situation adds a certain amount of water in visual response device, to keep material energy uniform stirring, 70 points
Stop adding water after clock, continue without water in suspension in stirring to reactor, material is in paste-like, stops heating, is slowly added to 600g matter
The lye that concentration is 40% is measured to alkalize, it is stirring while adding, after measuring material pH value greater than 8, the degreasing of 20g rosin is added, continues to heat
To 120 DEG C, a certain amount of water is added depending on slurry consistency in reaction process, stops heating after reaction 180 minutes, material is down to room
Temperature, filters out mother liquor, and the pH value of the dilution heat of sulfuric acid tune acid that addition mass concentration is 3% to slurry is warming up to 50 between 6-8
DEG C material is followed by stirring and washing and (reacts the rosin soap to be formed with alkali using rosin to wash), wash time is greater than 30 points
Clock, a certain amount of sodium hypochlorite progress bleaching is then added, and (additional amount of sodium hypochlorite is effective chlorine in material in 0.05-
Between 0.1g/100g, bleaching time is depending on requiring product whiteness), it then filters, filtered material uses 600ml every time
It is washed respectively 5 times added with 40 DEG C of hot water of siloxane polymer, total wash time is 30 minutes, filtering, by filtered object
Material is put into 70 DEG C of drier and dries to get the wood fibre with hydrophobic function.
Embodiment 2
By sawdust drying, it crushed 60 meshes, drying to constant weight at a temperature of 105 DEG C for screenings continuation, takes drying sawdust
70 meshes are crossed, takes the lower wood dust 100g of sieve to be put into reactor, 500g water is added, is gradually added 3g mass concentration after mixing evenly
For 98% the concentrated sulfuric acid be acidified, add sulfuric acid process needs be stirred continuously, prevent cellulose powder to be carbonized, measure its ph value 1-5 it
Between, reactor is heated to 110 DEG C, and be stirred continuously, moisture evaporation situation adds a certain amount of water in visual response device, to keep object
Material energy uniform stirring, stopping plus water after 100 minutes continue without water in suspension in stirring to reactor, and material is in paste-like, and stopping adds
Heat, be slowly added to 500g mass concentration be 50% lye alkalize, it is stirring while adding, measure material pH value be greater than 8 after, be added
Loose 30g perfume (or spice) degreasing continues to be heated to 130 DEG C, a certain amount of water is added depending on slurry consistency in reaction process, after reaction 200 minutes
Stop heating, material is down to room temperature, filter out mother liquor, the pH value that the dilution heat of sulfuric acid that mass concentration is 3% adjusts slurry is added
It between 6-8, is warming up to 60 DEG C and material is followed by stirring and washing, wash time is greater than 30 minutes, is then added a certain amount of time
Sodium chlorate carries out bleaching, and (additional amount of sodium hypochlorite is that effective chlorine is between 0.05-0.1g/100g in material, when bleaching
Between depending on to product whiteness require depending on), then filter, filtered material uses 700ml added with 8% siloxane polymer every time
60 DEG C of hot water wash 4 times respectively, and total wash time is 40 minutes, and filtered material is put into 110 DEG C of drier by filtering
Middle drying is to get the wood fibre with hydrophobic function.
Embodiment 3
By sawdust drying, it crushed 60 meshes, drying to constant weight at a temperature of 120 DEG C for screenings continuation, takes drying sawdust
70 meshes are crossed, takes the lower wood dust of sieve to be put into reactor, often takes 100g wood dust that 600g water is added, be gradually added after mixing evenly
The concentrated sulfuric acid that 2.5g mass concentration is 98% is acidified, and is added sulfuric acid process needs to be stirred continuously, is prevented cellulose powder to be carbonized, measure it
Ph value is heated to 100 DEG C between 1-5, by reactor, and is stirred continuously, and moisture evaporation situation is added a certain amount of in visual response device
Water keeps material energy uniform stirring, stops adding water after 80 minutes, continues without water in suspension in stirring to reactor, material is in slurry
Shape stops heating, is slowly added to the lye that 700g mass concentration is 36% and alkalizes, stirring while adding, measures material pH value greater than 8
Afterwards, the degreasing of 35g rosin is added, continues to be heated to 140 DEG C, adds a certain amount of water, reaction 240 depending on slurry consistency in reaction process
Stop heating after minute, material is down to room temperature, filter out mother liquor, the dilution heat of sulfuric acid tune acid that mass concentration is 2.5% is added extremely
Slurry pH value is warming up to 70 DEG C and material is followed by stirring and washing between 6-8, and wash time is greater than 30 minutes, is then added one
Quantitative sodium hypochlorite carry out bleaching (additional amount of sodium hypochlorite be in material effective chlorine 0.05-0.1g/100g it
Between, bleaching time is depending on requiring product whiteness), it then filters, filtered material uses 900ml added with 9% siloxanes every time
70 DEG C of hot water of polymer wash 3 times respectively, and total wash time is 30 minutes, and filtered material is put into 120 DEG C by filtering
Drier in drying to get the wood fibre with hydrophobic function.
Two, performance test
Be added to by the gypsum base putty of no addition wood fibre and respectively wood fibre that embodiment 1,2,3 obtains,
The gypsum base putty of commercially available wood fibre carries out the contrasting detection of properties, and the additive amount of wood fibre is dry powder total amount
0.6%, the result is as follows:
The test result of 1 wood fibre of table
As can be seen from the above table, the gypsum product for the wood fibre that addition 1-3 of the embodiment of the present invention is obtained, anti-folding, resistance to compression
Intensity is bigger, and water absorption is lower, and can be seen that the wood fibre obtained added with preparation method of the present invention from Fig. 1, Fig. 2
Gypsum product cracks less after dry.Wood fibre of the invention is equally applicable to be added to concrete mortar.
Claims (8)
1. a kind of preparation method with hydrophobic wood fibre, in turn includes the following steps:
(1) lignocellulose raw material dried, crush, cross 60 meshes, drying to constant weight at 60-130 DEG C for screenings, after 70 mesh
Sieve, obtains lignocellulose；
(2) lignocellulose and water are put into reactor for 1:4-6 in mass ratio, are gradually added wooden fibre after mixing evenly
The concentrated sulfuric acid for tieing up plain silty amount 2-5% is acidified, and enriching sulfuric acid process is stirred continuously, and prevents cellulose powder to be carbonized, by reactor
It is heated to 80-120 DEG C and is stirred continuously, moisture evaporation situation adds a certain amount of water in whipping process visual response device, to keep
Material energy uniform stirring stopped adding water after 60-120 minutes, continues stirring to material in paste-like, stops heating；
(3) lye for being slowly added to 4-7 times of lignocellulose quality alkalizes, stirring while adding, measures the pH value of material
When greater than 8, the rosin that 0.2-1 times of lignocellulose quality is added carries out degreasing, continues to be heated to 120-160 DEG C, react
The appropriate water supplement of slurry consistency is regarded in journey, to keep material energy uniform stirring, is reacted 180-240 minutes, is stopped heating；
(4) material is down to room temperature, filters out mother liquor, the pH value of dilute acid soln adjusting material is added between 6-8, heat temperature raising
Material is followed by stirring and washing to 50-70 DEG C, wash time is greater than 30 minutes, then is washed with the hot water added with siloxanes
It washs, the mass concentration of siloxanes aqueous solution is 5%-10%, and hot water temperature controls at 40-70 DEG C；
(5) it will be put into 110 DEG C of drier and dried to get the wood fibre with hydrophobic function after material filtering.
2. the preparation method with hydrophobic wood fibre according to claim 1, it is characterised in that: the preparation side
In method, the lignocellulose raw material of step (1) is waste wood or weedtree.
3. the preparation method with hydrophobic wood fibre according to claim 2, it is characterised in that: its feature exists
In: in the preparation method, the number for using siloxanes hot water to wash in step (4) is 2-5 time, the use of each siloxanes hot water
Amount is 500-1000ml, and total wash time is greater than 30 minutes.
4. the preparation method with hydrophobic wood fibre according to claim 3, it is characterised in that: the preparation side
In method, before step (4) carries out the washing of siloxanes hot water to material, sodium hypochlorite is first added and carries out bleaching, sodium hypochlorite
Additional amount is effective chlorine in material between 0.05-0.1g/100g.
5. -4 any preparation method with hydrophobic wood fibre according to claim 1, it is characterised in that: the preparation side
In method, the concentrated sulfuric acid of step (2) is the concentrated sulfuric acid that commercial available quality concentration is 98%.
6. the preparation method with hydrophobic wood fibre according to claim 5, it is characterised in that: the preparation side
In method, the lye of step (3) is to be dissolved to be formed by solid sodium hydroxide or potassium hydroxide, and lye mass concentration is 20%-56%.
7. the preparation method with hydrophobic wood fibre according to claim 6, it is characterised in that: the preparation side
In method, the diluted acid of step (4) is the dilute sulfuric acid that mass concentration is 2%-5%.
8. a kind of have hydrophobic function by what any preparation method with hydrophobic wood fibre of claim 1-7 obtained
It can wood fibre.
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| CA2424377C (en) * | 2000-10-04 | 2013-07-09 | Donald J. Merkley | Fiber cement composite materials using sized cellulose fibers |
| CN101565915B (en) * | 2009-04-30 | 2010-12-29 | 齐共水 | Process for producing enhanced wood fiber sponge |
| US9056792B2 (en) * | 2011-06-30 | 2015-06-16 | Weyerhaeuser Nr Company | Internally curing cement based materials |
| CN103483456B (en) * | 2013-10-15 | 2016-03-30 | 湖北博斐逊生物新材料有限公司 | A kind of preparation method of cement fiber sizing and the application in cement products thereof |
| CN106147259B (en) * | 2015-04-08 | 2019-02-15 | 中国科学院理化技术研究所 | A kind of preparation method and sheet-like fiber element of surface hydrophobicity sheet-like fiber element |
| CN106810613A (en) * | 2017-01-02 | 2017-06-09 | 胡云 | A kind of preparation method of hydrophobically modified nano-cellulose |
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