CN109745954A - A kind of preparation method of bluish dogbane adsorbent material - Google Patents
A kind of preparation method of bluish dogbane adsorbent material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of bluish dogbane adsorbent material, comprising the following steps: the soda boiling degumming in lye by bluish dogbane raw ramie；It is first impregnated after the completion with low-concentration alkali liquor, rear pure water rinsing is simultaneously dried；For bluish dogbane in organic acid, water-bath takes out bluish dogbane after 10g pretreatment is added；It is rinsed again with acetic acid or anhydride solution, reusable heat water rinses, drying for standby, and carries out absorption confirmatory experiment；Appropriate modified bluish dogbane is weighed, is added in methylene blue solution, water bath with thermostatic control oscillation takes supernatant liquor, measures absorbance, compare methylene blue solution standard curve, is verified qualified carboxy-modified bluish dogbane adsorbent material；This method makes bastose be utilized effectively, the biological adsorption material of production, product is porous, tightness is high, by acetic acid or anhydride modified processing, a large amount of carboxylic groups are introduced in bastose molecule, adsorptivity is preferable, for adsorbance up to 75~85mg/g, bastose adsorption efficiency is more than 90%.
Description
Technical field
The present invention relates to the preparation technical field of biological adsorption material, and in particular to a kind of preparation side of bluish dogbane adsorbent material
Method.
Background technique
Cellulose is the renewable resource of original and rich reserves on the current earth, it is present in plant cell membrane, bark,
Cotton fiber, fibre of flax for textile material, cereal skin or other plant, in recent years, it has been found that can also be with by the enzymolysis process of bacterium
Generate cellulose.Natural fiber can be classified as seed, skin, leaf and fruit.In composite material application, it is commonly used
It is the skin and leaf of plant, and the plant rich in this bast fiber has mainly various crudefiber crops, such as hemp, jute, flax, ramie
Fiber crops and mestha, have sisal hemp and banana rich in leaf fibre.
Bluish dogbane is Malvaceae Hibiscus annual herb bast fibre plant, is commonly called as mestha, gombo hemp, clock fiber crops, scientific name hemp
The rose of Sharon, Hibiscus cannabinus, growth period about 120~150 days.As jute, bluish dogbane stem bone is by bast and xylem
Two parts composition, kenaf phloem weight account for about 30%~40%, bast fiber cell length about 2.6mm or so and jute phase
Than bluish dogbane biological yield is high, and the requirement to soil is low, and management is simple, wide adaptability.Bastose is coarse, stiffening, spinnability
Difference, general number are 1.5~3Nm, are at most also no more than 10Nm, can only slightly prop up dilute knit.Bluish dogbane is as a kind of natural fiber material
Material, the internal structure and chemical composition of fiber determine the intensity that fiber shown, resistance coefficient, ultimate tensile strength and rise
Beginning modulus.The superior structural of natural fiber make its show outstanding tensile strength and modulus, durable, heap density it is very low,
Plasticity is strong and recyclable regenerative.Just because of bastose composed structure and substance characteristics the features such as, allow to be changed
Property become it is a kind of it is cheap, adsorption capacity is strong, biodegradable, high mechanical strength, compared with other natural cellulosic materials in life
Object adsorbent application aspect has apparent advantage.
Although natural bluish dogbane has certain adsorption capacity to organic pollutant as adsorbent material, adsorption effect is simultaneously paid no attention to
Think, and by being modified to it, i.e., introducing the functional group for having good affinity to organic pollutant on surface then can be with
Greatly improve the adsorption capacity of bluish dogbane.
Contain great amount of hydroxy group carboxyl isoreactivity group in natural cellulosic materials structure, being modified to it can be had
There is the cellulose derivative of specific function, reference can be provided to solve energy problem and environmental problem.Cellulose is fibrous, more
The natural polymer of capillary.Therefore has the characteristics that porous and large specific surface area, although hydroxyl has one containing there are many in molecule
Fixed adsorptivity.But the adsorption capacity of natural fiber is not strong.It can be drawn by a series of derivatization reaction of hydroxyl in molecule
People has the functional group of absorption property.Cellulose is set to contain more high adsorptivity groups, to improve its ion adsorption capacity.
Many different types of functional groups that metal ion is removed from aqueous solution are had studied at present, such as schiff bases, thiosemicarbazides, first
Acid, phosphoric acid and sulfonic acid etc..It is introduced by the derivative chemical reaction of hydroxyl to some groups in solution with ion with adsorption capacity,
Such as the anionic groups such as carboxyl, phosphate, sulfonic group, obtain cellulose derivative can with GOLD FROM PLATING SOLUTION category cationoid reaction,
Here it is with ion adsorbent.It is on the one hand due to bluish dogbane physically hole with higher as the research of adsorbent material
With metal ion physical absorption can occur for porosity and biggish surface area；On the other hand, bluish dogbane is rich in cellulose, hemicellulose
Element and lignin, pectin contain a large amount of functional group in the molecular structure of these ingredients, can pass through ion exchange, chelating
Etc. modes adsorb, be a kind of good biomass adsorbent.
There are many hydroxyls and acetic acid that esterification can occur in cellulose, acetic acid is dehydrated into acid anhydrides under concentrated sulfuric acid effect,
It is reacted with acid anhydrides with hydroxyl in cellulose, esterification can also occur with phenols (lignin).And cellulose can be with acetic acid shape
Circlewise acid anhydrides, to improve the degree that esterification combines.Acetic acid modification can introduce a large amount of carboxyl on the surface of bluish dogbane, greatly improve
The adsorption capacity of bastose.And being modified bastose is a kind of natural macromolecule modification material with rich space gap structure
Material can be difficult to the organic molecule degraded in effective absorption effluent, have preferable effect for handling dyeing waste water and leather-making waste water
Fruit.The modification of native cellulose is exactly to pass through the functional group for chemically reacting and introducing in cellulosic structure and having specific function, is obtained
There must be the new material of certain function, to greatly improve the application value and use value of natural cellulosic materials.
Natural biological adsorbent material such as bluish dogbane, jute raw ramie fiber is very limited to the adsorption capacity of sewage, and other
The problems such as big, inconvenient application that there are flow resistances when granulated adsorbent material is applied and more difficult recycling, and fibrous adsorbent material makes because of it
With form freedom degree it is big the features such as be widely used, existing modification technology such as 4- (- 2- pyridylazo) resorcinol group bluish dogbane system
The poisonous and harmful reagent auxiliary agent that standby and chloropropane modification-active ring oxygroup the methods of introducing is related to is more, has but violated ring
Protect the original intention of ecology.
Summary of the invention
For the present invention precisely in order to overcome above-mentioned deficiency, the technical problem to be solved is that provide a kind of bluish dogbane adsorbent material
Preparation method uses reproducible biomass bastose material, using the chemistry without side-effects to environment during the preparation process
Reagent is modified processing to it, obtains larger adsorption efficiency, is prepared into economic and environment-friendly, biodegradable new adsorbent
Material.
It is an object of the invention to propose that a kind of utilization acetic acid is modified the natural fibers such as bluish dogbane to produce life of good performance
The preparation method of object adsorbent is reacted using acetic acid carboxyl with hydroxyl in cellulose, and cellulose can form cyclic acid anhydride with acetic acid,
To improve the degree that esterification combines；Acetic acid modification can introduce a large amount of carboxyl on the surface of bluish dogbane, greatly improve bastose
Chemical adsorption capacity；Manufacture can natural degradation sewage adsorbent material, reduce chemical agent harm, make full use of biomass fiber
Resource turns waste into wealth, while can improve water quality again, effectively reduces pollution treatment cost；With renewable, at low cost, easy to operate, suction
The wide advantage of attached range.
Purpose to realize the present invention, the technical solution adopted is that: a kind of preparation method of bluish dogbane adsorbent material, the preparation
Method has specifically included following steps:
1) bluish dogbane lye degumming: bluish dogbane raw ramie is placed in mixed alkali liquor, and lye is warming up to 100 DEG C or 92~100
DEG C, soda boiling degumming is carried out under normal pressure or reduced pressure, the control of soda boiling usually time controls soda boiling degumming bath ratio in 1.5~2h
1:20；
Component and its concentration in mixed alkali liquor are as follows: NaOH 10~15%, NaHCO33~5%, penetrating agent JFC 1~
2% (o.w.f is relative to bluish dogbane quality), Na2SiO3Or NaAlO2(o.w.f is relative to bluish dogbane quality) 1.5~3%, tripolyphosphate
Sodium (o.w.f is relative to bluish dogbane quality) 1.5~3% and NaClO or NaBrO 0.5~1.5%；Wherein auxiliary agent sodium metasilicate or inclined aluminium
Sour sodium can keep the concentration of alkali, be hydrolyzed into silicic acid or alumine hydroxide colloid or ion, prevent pigment deposition, improve the white of degummed ramie
Degree；Sodium tripolyphosphate has infiltration, diffusion, emulsification, increases the surface-active of kiering liquid, convenient for bastose and colloid point
From, while preventing pigment deposition on fiber；Fibre morphology made from degumming is preferable, and degumming rate is up to 25~30%；
After the completion of soda boiling degumming, the bluish dogbane of soda boiling degumming is pulled out, first soaks bluish dogbane in 40~70 DEG C of low-concentration alkali liquors
60~90min is steeped, then is rinsed bluish dogbane 2~3 times with 10~30 DEG C of low-temperature pure water, is dried；
The component and its concentration of low-concentration alkali liquor are as follows: NaOH 3~5%, NaHCO31~3% and Na2SiO3Or
NaAlO20.5~1.5%；
2) modified with organic acids: 36% acetic acid 20ml is diluted to 4~8% solution or maleic anhydride 20ml is diluted to
4~6% solution or 36% acetic anhydride 20ml dilution 2~6% solution or acyl chlorides 20ml be diluted to 3~8% solution,
25~35 DEG C of heated at constant temperature in water-bath are first placed in, the pretreated bluish dogbane of 10g is added, is placed in thermostat water bath, 35 DEG C
60~100min of lower reaction takes out bluish dogbane；
First with 5~10% acetum or 5~10% acetic acid anhydride solution or 5~10% maleic anhydride solution,
Or 5~10% acetic anhydride and the mixed solution of maleic anhydride rinse modified bluish dogbane, then with temperature are 35~55 DEG C of warm water
It impregnates, rinse modified bluish dogbane 2~3 times, 60 DEG C of freeze-day with constant temperature are spare, and carry out absorption confirmatory experiment；
3) methylene blue dye liquor standard concentration curve is drawn: being taken methylene blue dye particle that deionized water is added, is configured to
The methylene blue solution of 500mg/L, being diluted to concentration respectively is 5mg/L, 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/
L, 30min is placed after the methylene blue solution of 60mg/L shakes up makes the complete stability that develops the color；
It is that 664nm locates in wavelength, using distilled water as blank control every group of absorbance of measurement, according to being inhaled under various concentration
Light varience draws out absorbance-concentration standard working curve of methylene blue solution, and according to langbobier law, absorbance
A is directly proportional to concentration C, therefore concentration is set as x-axis, and absorbance A is y-axis, carries out linear fit to it, show that the work of its standard is bent
Line equation: A=0.0053C-0.0043；
4) absorption test: weigh 0.5~1g of carboxy-modified bluish dogbane adsorbent material, be added to 100ml concentration be 100~
200mg/L methylene blue solution, 150r/min 90~100min of constant temperature oscillation, takes in 80~85 DEG C of constant temperature oscillation water-bath
Supernatant liquor measures absorbance with spectrophotometer respectively, compares methylene blue solution standard curve, obtain supernatant,
When adsorbance reaches 75~85mg/g, and bastose adsorption efficiency is more than 90%, it is verified qualified carboxy-modified bluish dogbane
Adsorbent material.
The invention has the benefit that this preparation method can be such that low-cost bastose of abundant raw material etc. obtains effectively
It utilizes, produces the biological adsorption material of industrial wastewater, product is porous, and tightness is high, by acetic acid or anhydride modified processing, makes
Esterification occurs for alcoholic extract hydroxyl group and carboxyl or acid anhydrides in bastose element, to introduce a large amount of carboxyls in bastose molecule
Group；Adsorptivity is preferable, and for adsorbance up to 75~85mg/g, bastose adsorption efficiency is more than 90%.
Detailed description of the invention
Fig. 1 is methylene blue solution standard curve of the invention (concentration range: 0~60mg/L).
Fig. 2 is bluish dogbane raw ramie SEM figure (× 1000 times) of the invention.
Fig. 3 is bluish dogbane SEM figure (× 1000 times) after soda boiling of the invention.
Fig. 4 is that SEM schemes (× 500 times) to acetic acid before modified after degumming of the invention.
Fig. 5 is the modified SEM figure (× 500 times) of alkali process of the invention+acetic acid.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
Embodiment 1
It please refers to shown in Fig. 1-5, a kind of preparation method of bluish dogbane adsorbent material, the preparation method has specifically included following
Step:
1) bluish dogbane lye degumming: bluish dogbane raw ramie is placed in mixed alkali liquor, lye is warming up to 100 DEG C, in condition of normal pressure
Lower progress soda boiling degumming, the control of soda boiling usually time control soda boiling degumming bath ratio 1:20 in 1.5h；
Component and its concentration in mixed alkali liquor are as follows: NaOH 10%, NaHCO35%, (the o.w.f phase of penetrating agent JFC 1%
For bluish dogbane quality), Na2SiO3Or NaAlO2(o.w.f is relative to bluish dogbane quality) 2%, (o.w.f is relative to red for sodium tripolyphosphate
Numb quality) 2% and NaClO or NaBrO0.5%；
After the completion of soda boiling degumming, the bluish dogbane of soda boiling degumming is pulled out, first impregnates bluish dogbane in 70 DEG C of low-concentration alkali liquors
60min, then rinsed bluish dogbane 3 times with 10 DEG C of low-temperature pure water, it dries；
The component and its concentration of low-concentration alkali liquor are as follows: NaOH 5%, NaHCO32% and Na2SiO3Or NaAlO21%；
2) modified with organic acids: 36% acetic acid 20ml is diluted to 6% solution or maleic anhydride 20ml is diluted to 6%
Solution or 36% acetic anhydride 20ml dilution 6% solution or acyl chlorides 20ml be diluted to 6% solution, be first placed in water-bath
In 25 DEG C of heated at constant temperature, add the pretreated bluish dogbane of 10g, be placed in thermostat water bath, 90min is reacted at 35 DEG C, take out
Bluish dogbane；
First with 10% acetum or 5% acetic acid anhydride solution or 5% maleic anhydride solution or 5% acetic acid
The mixed solution of acid anhydride and maleic anhydride rinses modified bluish dogbane, then the warm water for being 35 DEG C with temperature impregnates, rinses modified bluish dogbane 3
Secondary, 60 DEG C of freeze-day with constant temperature are spare, and carry out absorption confirmatory experiment；
3) methylene blue dye liquor standard concentration curve draws (see Fig. 1): taking methylene blue dye particle that deionization is added
Water, is configured to the methylene blue solution of 500mg/L, be diluted to respectively concentration be 5mg/L, 10mg/L, 20mg/L, 30mg/L,
The methylene blue solution of 40mg/L, 50mg/L, 60mg/L, which place 30min after shaking up, makes the complete stability that develops the color；
It is that 664nm locates in wavelength, using distilled water as blank control every group of absorbance of measurement, according to being inhaled under various concentration
Light varience draws out absorbance-concentration standard working curve of methylene blue solution, and according to langbobier law, absorbance
A is directly proportional to concentration C, therefore concentration is set as x-axis, and absorbance A is y-axis, carries out linear fit to it, show that the work of its standard is bent
Line equation: A=0.0053C-0.0043；
4) absorption test: weighing carboxy-modified bluish dogbane adsorbent material 1g, and the concentration for being added to 100ml is 100mg/L methylene
Base indigo plant solution, 150r/min constant temperature oscillation 90min, takes supernatant liquor, uses spectrophotometric in 80 DEG C of constant temperature oscillation water-bath
Meter measures absorbance respectively, compares methylene blue solution standard curve, obtains supernatant, when adsorbance reaches 80mg/g,
When bastose adsorption efficiency reaches 91% or more, it is verified qualified carboxy-modified bluish dogbane adsorbent material.
Embodiment 2
It please refers to shown in Fig. 1-5, a kind of preparation method of bluish dogbane adsorbent material, the preparation method has specifically included following
Step:
1) bluish dogbane lye degumming: bluish dogbane raw ramie is placed in mixed alkali liquor, lye is warming up to 100 DEG C, in condition of normal pressure
Lower progress soda boiling degumming, the control of soda boiling usually time control soda boiling degumming bath ratio 1:20 in 2h；
Component and its concentration in mixed alkali liquor are as follows: NaOH 10%, NaHCO35%, (the o.w.f phase of penetrating agent JFC 1%
For bluish dogbane quality), Na2SiO3Or NaAlO2(o.w.f is relative to bluish dogbane quality) 1.5%, sodium tripolyphosphate (o.w.f relative to
Bluish dogbane quality) 1.5% and NaClO or NaBrO 1.5%；
After the completion of soda boiling degumming, the bluish dogbane of soda boiling degumming is pulled out, first impregnates bluish dogbane in 50 DEG C of low-concentration alkali liquors
60min, then rinsed bluish dogbane 3 times with 20 DEG C of low-temperature pure water, it dries；
The component and its concentration of low-concentration alkali liquor are as follows: NaOH 3%, NaHCO31% and Na2SiO3Or NaAlO20.5%；
2) modified with organic acids: 36% acetic acid 20ml is diluted to 8% solution or maleic anhydride 20ml is diluted to 4%
Solution or 36% acetic anhydride 20ml dilution 6% solution or acyl chlorides 20ml be diluted to 5% solution, be first placed in water-bath
In 25 DEG C of heated at constant temperature, add the pretreated bluish dogbane of 10g, be placed in thermostat water bath, 90min is reacted at 35 DEG C, take out
Bluish dogbane；
First with 10% acetum or 5% acetic acid anhydride solution or 10% maleic anhydride solution or 5% acetic acid
The mixed solution of acid anhydride and maleic anhydride rinses modified bluish dogbane, then the warm water for being 35 DEG C with temperature impregnates, rinses modified bluish dogbane 2
Secondary, 60 DEG C of freeze-day with constant temperature are spare, and carry out absorption confirmatory experiment；
3) methylene blue dye liquor standard concentration curve draws (see Fig. 1): taking methylene blue dye particle that deionization is added
Water, is configured to the methylene blue solution of 500mg/L, be diluted to respectively concentration be 5mg/L, 10mg/L, 20mg/L, 30mg/L,
The methylene blue solution of 40mg/L, 50mg/L, 60mg/L, which place 30min after shaking up, makes the complete stability that develops the color；
It is that 664nm locates in wavelength, using distilled water as blank control every group of absorbance of measurement, according to being inhaled under various concentration
Light varience draws out absorbance-concentration standard working curve of methylene blue solution, and according to langbobier law, absorbance
A is directly proportional to concentration C, therefore concentration is set as x-axis, and absorbance A is y-axis, carries out linear fit to it, show that the work of its standard is bent
Line equation: A=0.0053C-0.0043；
4) absorption test: weighing carboxy-modified bluish dogbane adsorbent material 1g, and the concentration for being added to 100ml is 200mg/L methylene
Base indigo plant solution, 150r/min constant temperature oscillation 95min, takes supernatant liquor, uses spectrophotometric in 80 DEG C of constant temperature oscillation water-bath
Meter measures absorbance respectively, compares methylene blue solution standard curve, obtains supernatant, when adsorbance reaches 82mg/g,
When bastose adsorption efficiency reaches 90.5%, it is verified qualified carboxy-modified bluish dogbane adsorbent material.
Embodiment 3
It please refers to shown in Fig. 1-5, a kind of preparation method of bluish dogbane adsorbent material, the preparation method has specifically included following
Step:
1) bluish dogbane lye degumming: bluish dogbane raw ramie is placed in mixed alkali liquor, lye is warming up to 92 DEG C, in reduced pressure
Lower progress soda boiling degumming, the control of soda boiling usually time control soda boiling degumming bath ratio 1:20 in 1.5h；
Component and its concentration in mixed alkali liquor are as follows: NaOH 15%, NaHCO35%, (the o.w.f phase of penetrating agent JFC 2%
For bluish dogbane quality), Na2SiO3Or NaAlO2(o.w.f is relative to bluish dogbane quality) 3%, (o.w.f is relative to red for sodium tripolyphosphate
Numb quality) 3% and NaClO or NaBrO0.5%；
After the completion of soda boiling degumming, the bluish dogbane of soda boiling degumming is pulled out, first impregnates bluish dogbane in 40 DEG C of low-concentration alkali liquors
60min, then rinsed bluish dogbane 3 times with 30 DEG C of low-temperature pure water, it dries；
The component and its concentration of low-concentration alkali liquor are as follows: NaOH 5%, NaHCO33% and Na2SiO3Or NaAlO21.5%；
2) modified with organic acids: 36% acetic acid 20ml is diluted to 8% solution or maleic anhydride 20ml is diluted to 6%
Solution or 36% acetic anhydride 20ml dilution 6% solution or acyl chlorides 20ml be diluted to 8% solution, be first placed in water-bath
In 30 DEG C of heated at constant temperature, add the pretreated bluish dogbane of 10g, be placed in thermostat water bath, 80min is reacted at 35 DEG C, take out
Bluish dogbane；
First with 10% acetum or 10% acetic acid anhydride solution or 10% maleic anhydride solution or 5% vinegar
The mixed solution of acid anhydrides and maleic anhydride rinses modified bluish dogbane, then the warm water for being 55 DEG C with temperature impregnate, rinse it is modified red
Fiber crops 3 times, 60 DEG C of freeze-day with constant temperature are spare, and carry out absorption confirmatory experiment；
3) methylene blue dye liquor standard concentration curve draws (see Fig. 1): taking methylene blue dye particle that deionization is added
Water, is configured to the methylene blue solution of 500mg/L, be diluted to respectively concentration be 5mg/L, 10mg/L, 20mg/L, 30mg/L,
The methylene blue solution of 40mg/L, 50mg/L, 60mg/L, which place 30min after shaking up, makes the complete stability that develops the color；
It is that 664nm locates in wavelength, using distilled water as blank control every group of absorbance of measurement, according to being inhaled under various concentration
Light varience draws out absorbance-concentration standard working curve of methylene blue solution, and according to langbobier law, absorbance
A is directly proportional to concentration C, therefore concentration is set as x-axis, and absorbance A is y-axis, carries out linear fit to it, show that the work of its standard is bent
Line equation: A=0.0053C-0.0043；
4) absorption test: weighing carboxy-modified bluish dogbane adsorbent material 1g, and the concentration for being added to 100ml is 150mg/L methylene
Base indigo plant solution, 150r/min constant temperature oscillation 100min, takes supernatant liquor, uses spectrophotometric in 85 DEG C of constant temperature oscillation water-bath
Meter measures absorbance respectively, compares methylene blue solution standard curve, supernatant is obtained, when adsorbance reaches 84.5mg/
G when bastose adsorption efficiency reaches 92.8%, is verified qualified carboxy-modified bluish dogbane adsorbent material.
Key of the invention is due to bluish dogbane physically porosity with higher and biggish surface area, to bluish dogbane
Raw ramie carries out soda boiling treatment process, then carries out the acetic acid or anhydride modified of bluish dogbane, and bluish dogbane after modified to methylene
The adsorptivity of blue dye liquor is tested, chemical agent small toxicity used in entire treatment process, cheap, easy to operate, is utilized
The porous property of bastose, content of cellulose is higher, the hydroxyl isopolarity group on surface can with acetic acid esterified and introduce more
Carboxyl, be greatly improved bastose to the adsorption efficiency of methylene blue sewage, meanwhile, reduce at dyeing waste water or sewage
Cost is managed, bluish dogbane adsorbent material itself is nontoxic, biodegradable, no pollution to the environment.Acetic acid and reactive anhydride and fibre
It ties up and forms ester bond between plain hydroxyl, and carboxyl is introduced into cellulose, be easy to Liquidity limit dyestuff and metal cation.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (9)
1. a kind of preparation method of bluish dogbane adsorbent material, it is characterised in that: the preparation method has specifically included following steps:
1) bluish dogbane lye degumming: bluish dogbane raw ramie is placed in mixed alkali liquor, and lye is warming up to 100 DEG C or 92~100 DEG C,
Soda boiling degumming is carried out under normal pressure or reduced pressure, the control of soda boiling usually time controls soda boiling degumming bath ratio 1:20 in 1.5~2h；
After the completion of soda boiling degumming, the bluish dogbane of soda boiling degumming is pulled out, bluish dogbane is first impregnated 60 in 40~70 DEG C of low-concentration alkali liquors
~90min, then rinsed bluish dogbane 2~3 times with 10~30 DEG C of low-temperature pure water, it dries；
2) modified with organic acids: configured organic acid is first placed in 25~35 DEG C of heated at constant temperature in water-bath, it is pre- to add 10g
Treated bluish dogbane, is placed in thermostat water bath, and 60~100min is reacted at 35 DEG C, takes out bluish dogbane；
Modified bluish dogbane is rinsed with 5~10% acetic acid or anhydride solution, then the warm water for being 35~55 DEG C with temperature is impregnated, rinsed
Modified bluish dogbane 2~3 times, 60 DEG C of freeze-day with constant temperature are spare, and carry out absorption confirmatory experiment；
3) methylene blue dye liquor standard concentration curve is drawn: being taken methylene blue dye particle that deionized water is added, is configured to
The methylene blue solution of 500mg/L, being diluted to concentration respectively is 5mg/L, 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/
L, 30min is placed after the methylene blue solution of 60mg/L shakes up makes the complete stability that develops the color；
It is every group of absorbance to be measured as blank control using distilled water, according to absorbance under various concentration at 664nm in wavelength
Absorbance-concentration standard working curve of methylene blue solution is drawn out in variation, and according to langbobier law, absorbance A with
Concentration C is directly proportional, therefore concentration is set as x-axis, and absorbance A is y-axis, carries out linear fit to it, obtains its standard working curve
Equation: A=0.0053C-0.0043；
4) absorption test: weigh 0.5~1g of carboxy-modified bluish dogbane adsorbent material, be added to 100ml concentration be 100~
200mg/L methylene blue solution, 150r/min 90~100min of constant temperature oscillation, takes in 80~85 DEG C of constant temperature oscillation water-bath
Supernatant liquor measures absorbance with spectrophotometer respectively, compares methylene blue solution standard curve, obtain supernatant,
When adsorbance reaches 75~85mg/g, and bastose adsorption efficiency is more than 90%, it is verified qualified carboxy-modified bluish dogbane
Adsorbent material.
2. a kind of preparation method of bluish dogbane adsorbent material according to claim 1, it is characterised in that: the preparation method step
The component and its concentration in mixed alkali liquor in rapid 1 are as follows: NaOH 10~15%, NaHCO33~5%, penetrating agent JFC 1~
2% (o.w.f is relative to bluish dogbane quality), Na2SiO3Or NaAlO2(o.w.f is relative to bluish dogbane quality) 1.5~3% and trimerization phosphorus
Sour sodium (o.w.f is relative to bluish dogbane quality) 1.5~3%.
3. a kind of preparation method of bluish dogbane adsorbent material according to claim 1 or 2, it is characterised in that: the preparation side
Further include in mixed alkali liquor in method step 1 have concentration be 0.5~1.5% NaClO or NaBrO.
4. a kind of preparation method of bluish dogbane adsorbent material according to claim 1, it is characterised in that: the preparation method step
The component and its concentration of low-concentration alkali liquor in rapid 1 are as follows: NaOH 3~5%, NaHCO31~3% and Na2SiO3Or NaAlO2 0.5
~1.5%.
5. a kind of preparation method of bluish dogbane adsorbent material according to claim 1, it is characterised in that: the preparation method step
The acetic acid 20ml that organic acid in rapid 2 is 36% is diluted to 4~8% solution.
6. a kind of preparation method of bluish dogbane adsorbent material according to claim 1, it is characterised in that: the preparation method step
Organic acid in rapid 2 is the solution that maleic anhydride 20ml is diluted to 4~6%.
7. a kind of preparation method of bluish dogbane adsorbent material according to claim 1, it is characterised in that: the preparation method step
The solution for the acetic anhydride 20ml dilution 2~6% that organic acid in rapid 2 is 36%.
8. a kind of preparation method of bluish dogbane adsorbent material according to claim 1, it is characterised in that: the preparation method step
Organic acid in rapid 2 is the solution that acyl chlorides 20ml is diluted to 3~8%.
9. a kind of preparation method of bluish dogbane adsorbent material according to claim 1, it is characterised in that: the preparation method step
Acid anhydrides in rapid 2 is the mixture of acetic anhydride, maleic anhydride or both.
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| CN114728851A (en) * | 2019-10-23 | 2022-07-08 | 红麻投资有限公司 | Building material and method for producing same |
| CN115739035A (en) * | 2022-12-05 | 2023-03-07 | 南京信息工程大学 | Method for modifying kenaf straws by succinic anhydride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114728851A (en) * | 2019-10-23 | 2022-07-08 | 红麻投资有限公司 | Building material and method for producing same |
| CN115739035A (en) * | 2022-12-05 | 2023-03-07 | 南京信息工程大学 | Method for modifying kenaf straws by succinic anhydride |
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