CN106000331A - Preparation method for cationic solid adsorption agent with old newspapers as raw material, product and application of product - Google Patents
Preparation method for cationic solid adsorption agent with old newspapers as raw material, product and application of product Download PDFInfo
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- CN106000331A CN106000331A CN201610223875.7A CN201610223875A CN106000331A CN 106000331 A CN106000331 A CN 106000331A CN 201610223875 A CN201610223875 A CN 201610223875A CN 106000331 A CN106000331 A CN 106000331A
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- old newspaper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
- B01J2220/4831—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton having been subjected to further processing, e.g. paper, cellulose pulp
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method for a cationic solid adsorption agent with old newspapers as raw material, a product and an application of the product, wherein the method comprises the following steps: tearing the old newspapers into pieces, soaking for 24 h in water, beating, and then centrifuging; carrying out one-time deinking: according to the mass percentage, with the paper pulp concentration of 8% and the sodium sulfite amount of 4%, adjusting the pH value to 6-7, and soaking for 75 min at the temperature of 60-70 DEG C; centrifuging and drying the old newspapers, and carrying out secondary deinking: with the paper pulp concentration of 5%, with the NaOH amount of 0.6%, with the H2O2 amount of 0.9%, and at the temperature of 50 DEG C, soaking for 60 min; drying the paper pulp to constant weight at the temperature of 50 DEG C, and putting into a dryer for standby application; adding a phosphoric acid solution, and carrying out a stirring reaction for 2 h at room temperature; draining the liquid, then drying to no water, rising the temperature to 120 DEG C, and heating for 1.5 h; washing to be neutral with deionized water; and drying to constant weight. The phosphoric acid modified paper particles prepared by the process have both excellent physical adsorption properties and excellent chemical adsorption properties, especially have the adsorption properties on cation in water, and have the adsorption performance greatly improved after modification.
Description
Technical field
The invention belongs to material modified technical field, be specifically related to a kind of old newspaper as the preparation method of the cation solid absorbent of raw material and product and application.
Background technology
Absorption is a kind of cheap effective processing mode.Document report adsorbent species is a lot, has lignin, acid treatment sintering laterite, modified SWCN, acrylic acid modified starch, activated carbon, the modified layered magnesium silicate of aminopropyl, tripolycyanamide/copolymer-maleic anhydride, eggshell, activated carbon supported stannum oxide, Pericarppium arachidis hypogaeae etc..The response rate of China's waste paper only has about 43.8%, and the waste paper reclaimed uses mainly as paper making raw material, and purposes is the most single.And old newspaper amount is big, low cost, can be as cellulose modified use after deinking.
Chinese patent 201110075095.X discloses a kind of with NaOH, NaSiO3, and detergent and hydrogen peroxide as deinking agent, newspaper pulp carried out deinking, then the method that a kind of old newspaper of drying processes waste water as solid absorbent.Chinese patent 201110075095.X disclose a kind of using sodium hydroxide solution and sodium silicate solution as modifying agent, hydrogen peroxide and detergent as the preparation method of a kind of newspaper pulp solid adsorbent of deinking agent.Chinese patent 201210049807.5 disclose a kind of by after newspaper deinking using epoxychloropropane and triethylamine as a kind of anionic dye adsorbent method of modifying agent and application thereof.Above-mentioned sorbent preparation method mainly to the fiber of the old and useless newspaper after deinking with half fiber is dried or the method such as modification is as solid absorbent, but, it is limited to the absorption property of water body cationic.
Summary of the invention
Instant invention overcomes shortcoming of the prior art, it is provided that a kind of old newspaper considerably increases the absorption property to water body cationic as the preparation method of the cation solid absorbent of raw material, modified old and useless newspaper.
In order to solve above-mentioned technical problem, the present invention is achieved by the following technical solutions:
A kind of old newspaper is as the preparation method of the cation solid absorbent of raw material, and it comprises the following steps:
(1) old newspaper tears to bits, is soaked in water 24 hours, centrifugal after making beating；
(2) deinking is carried out: according to mass percent, pulp density: 8%, sodium sulfite consumption: 4%, tune pH value is 6-7, temperature 60～70 DEG C of immersion 75min；
(3) the centrifugal and old newspaper of drying steps (2) gained, carries out secondary deinking: pulp density: 5%, NaOH consumption 0.6%, H2O2Consumption 0.9%, temperature 50 C, soaks 60min；
(4) paper pulp after secondary deinking is dried to constant weight at 50 DEG C, puts in exsiccator standby；
(5) weigh secondary de inked pulp, add 1mol/L phosphoric acid solution, stirring reaction 2h under room temperature；
(6) it is dried to exclusion at 50 DEG C after draining liquid, is warming up to 120 DEG C of heating 1.5h；
(7) with deionized water, the product of step (6) gained is washed to neutral；
(8) it is dried to constant weight at 50 DEG C.
Described old newspaper is torn into the fragment of 2 × 5cm.
In step (5), the ratio of described secondary de inked pulp and phosphoric acid solution is 1:5.
A kind of old newspaper modified product, prepares in accordance with the method for claim 1.
Old newspaper modified product is in the application prepared on water pollutant adsorbent
Compared with prior art, the invention has the beneficial effects as follows:
Phosphoric acid modification newspaper granule prepared by present invention process, has outstanding physical absorption performance and outstanding chemisorbed performance, the particularly absorption property to the cation in water simultaneously, and through modified, absorption property is greatly promoted.
Accompanying drawing explanation
Accompanying drawing is used for providing a further understanding of the present invention, is used for together with embodiments of the present invention explaining the present invention, is not intended that limitation of the present invention, in the accompanying drawings:
The IR spectrogram of Fig. 1 newspaper fiber；
A: unmodified；B: phosphorylation is modified.
Fig. 2 old newspaper fiber phosphorylation mechanism of modification；
The SEM of Fig. 3 phosphorylation modification old newspaper fiber；
A: old newspaper fiber (400 times) b: phosphorylation modification old newspaper fiber (400 times) c before unmodified: old newspaper fiber (5000 times) d: phosphorylation modification old newspaper fiber (5000 times) before unmodified
EDS collection of illustrative plates before and after Fig. 4 old newspaper modified phosphate.
A: before modified；B: modified
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is merely to illustrate and explains the present invention, is not intended to limit the present invention.
First old and useless newspaper is broken into the little scraps of paper, then the 24h that is soaked in water by the present invention, it is therefore an objective to remove the impurity foreign body inside the old and useless newspaper reclaimed, additionally sufficiently soak and can make the long-pending increase of paper plastochondria, structure softening, makes fiber separate, and disperse ink is conducive to follow-up deinking step.
After test, find that the old and useless newspaper after twice deinking compares the better of for once deinking, NaOH has been mainly saponification and regulation pH value in deinking process, it can make fibre swelling, makes resin in ink, sizing material easily be saponified by hydrabrusher mechanical friction effect.H2O2In the basic conditions, for the decolouring to coloring matter, make fiber bleach, and contribute to the removing of ink particle.But the deinking efficiency of how many couples of H2O2 of residual ink has a major impact, therefore, experiment uses NaSO3 to be removed by part ink under conditions of neutrality, then carries out second time deinking.
In 40 DEG C of water-baths, 2h is soaked with phosphoric acid solution after mixing, wherein phosphoric acid is middle strong acid, have more high dehydrated, plant cellulose molecular complex can be made to be partly dissolved, phosphate groups in phosphoric acid can be with grafting on cellulosic molecule, increase the active group on surface, preferred concentration of the present invention is the phosphoric acid of 1～2mol/L, it is modified causing modified effect the best less than the phosphoric acid of this value range when using, uses and be modified higher than the phosphoric acid solution of this value range, the burden of subsequent cleaning operation can be increased；
The product that step (5) obtains is drained, old newspaper granule is put into together with phosphoric acid first oven drying at low temperature in baking oven, it is warming up to 120 DEG C immediately and dries 1.5h, phosphoric acid at high temperature has certain dehydration property, the surface making old newspaper granule forms cellular, rough surface, meanwhile, under the high temperature conditions can be by PO4 3-Group grafting, on the cellulosic molecule of particle surface, is conducive to increasing the negative charge of particle surface, strengthens the electrostatic adsorption to cation.
The product of step (6) gained is washed with deionized to pH=7, due to the pH < H in water when 7+Ion can produce competitive Adsorption with the cation in water, proves in adsorption process through cation-adsorption Experimental comparison, as pH=7 most beneficial for the adsorption effect of old and useless newspaper granule.
The effect granule modified in order to verify old newspaper, is characterized it with FTIR and SEM, EDS.
Old newspaper through the modified fiber obtaining loosening of deinking and phosphorylation, its phosphorylation before modified after IR collection of illustrative plates as shown in Figure 1.Cellulosic structure contains OH, C-O-C ,-CH2-functional group, and on the IR figure of unmodified newspaper, analysis is learnt: 3424cm-1 is the oxygen hydrogen stretching vibration of-OH, and 2901 is the hydrocarbon stretching vibration of-CH2-, and 1428,1370 is the bending vibration of-CH2-.This is due to phosphorylated modified, and partly-OH esterification is phosphoric acid ester bond, as shown in Figure 2.The IR figure of modified fibre is substantially identical with unmodified fibers, shows that the agent structure of fiber is not corrupted, but occurs in that at 1050cm-1 as P-O series stretching vibration.Phosphorylated modified, cellulose side chain occurs in that phosphate ester anionic group, ion pair can be formed with cation malachite green oxalate and produce absorption, so that absorbability strengthens.
Its adsorption property is played a decisive role by the apparent condition after fibre modification, and Fig. 3 is the SEM figure of phosphorylation rear old newspaper fiber before modified.By Fig. 3 a it can be seen that before modified old newspaper fibre diameter be that about 100 μm, length is longer.And Fig. 3 b display modified fibre diameter of phosphorylation does not has significant change, but length shortens.By Fig. 3 c it can be seen that the smooth densification of fiber surface before modified, and fiber surface stratiform structure destroyed modified from Fig. 3 d, occurring that part is peeled off, surface texture loosens.SEM shows that phosphorylation has not only cut off fiber, also destroys surface layer, makes cellulose surface structure division Phosphation.There is the phosphate group of negative electricity on the loose and surface band of surface texture, all can greatly facilitate the absorption to cation.
And Fig. 4 is the EDS figure before and after old newspaper fibre modification.Old newspaper is after deinking processes, and Main Ingredients and Appearance is cellulose.But the old newspaper after deinking still contains metal and the nonmetalloid such as a small amount of Organic substance and calcium, sodium, magnesium, aluminum, silicon and sulfur.And phosphorylated modified, surface has detected the phosphorus of 0.52%, calcium and sulfur content and has substantially reduced, and sodium magnesium does not detects.Illustrate that phosphorylation modification has not only made on fiber surface band phosphate group, and significantly reduce other impurity content, eliminate the impact of different old newspaper difference.
The present invention is after old and useless newspaper is carried out secondary deinking, utilizes phosphoric acid to carry out high temperature modified to old and useless newspaper microgranule, improves its surface texture so that it is surface forms out-of-flatness and cavernous surface and increases specific surface area, improves its physical absorption performance；Additionally paper grain is dried under conditions of high temperature with phosphoric acid, by PO4 3-Ion grafting forms modified phosphate cellulose on paper grain surface fiber element molecule, because of its in water in negative electricity polarity, therefore, considerably increase the absorption property to water body cationic by the old and useless newspaper of phosphoric acid modification.
Material modified adsorption isotherm experiment
Langmuir equation at constant temperature is used for describing the liquid phase adsorption behavior that outer surface contains limited adsorption site, i.e. homogenizing absorption.And Freundlich equation at constant temperature is mainly used to describe heterogeneous body absorption.Using Langmuir and Freundlich equation at constant temperature to be fitted 15 DEG C, 25 DEG C and 35 DEG C of absorption results, fitting result and the parameter obtained are as shown in table 1.
Langmuir equation at constant temperature is:
Ce/qe=1/KLqm+Ce/qm (3)
In formula 3, Ce is adsorption equilibrium concentration, mg/L；Qe is equilibrium adsorption capacity, mg/g；Qm is monolayer saturated extent of adsorption, mg/g；KL is adsorption equilibrium costant, L/mg；Freundlich equation at constant temperature is:
Lnqe=lnKF+ (lnCe)/n (4)
In formula 4, KF represents the size of absorbability, and its numerical value the biggest expression absorbability is the biggest；And n represents the power of absorption motive force, numerical value is shown to be profitable absorption more than 1, is shown to be reciprocity absorption less than 1.
The result using Langmuir and Freundlich equation at constant temperature to be fitted the absorption situation of modified old newspaper fiber is as shown in table 2.
The Isothermal Model parameter of table 2 phosphoric acid modification old newspaper fibers adsorption malachite green oxalate
Material modified the adsorption kinetic data
In order to study absorption mechanism and control the speed of adsorption step, malachite green oxalate adsorption process on phosphoric acid modification old newspaper fiber is inquired into accurate two grades of equation kinetics model of biosorptions with pseudo-first-order equation herein.
Pseudo-first-order Lagergren equation: Log (qe–qt)=logqe–(k1/2.303)t
Q in formulaeAnd qtIt is respectively equilibrium adsorption capacity and t adsorbance, mg/g；k1Be as the criterion First-order equation adsorbing filament technique, L/min.
Accurate two grades of equations are: t/qt=1/ (k2qe 2)+t/qe
K in formula2The secondary absorption that is as the criterion speed constant, g/ (mg min)
Using pseudo-first-order equation model, equation of linear regression is Y=1.0028-0.008x
With accurate two grades of equation models, equation of linear regression is Y=0.0116x+0.0301
The pseudo-first-order equation that malachite green oxalate is adsorbed by the modified old newspaper fiber of table 3 and accurate two grades of equation parameters
As shown in Table 3, by the coefficient R of pseudo-second order kinetic equation simulation2Close to 1, and QeValue of calculation 86.20mg/g and experiment value 85.37mg/g closely, and the R of pseudo-first-order kinetics equation2Only 0.9053, QeThe biggest with experiment value difference.Hence it is demonstrated that adsorption process meets pseudo-second order kinetic equation, site is more accessible saturated, is the complex effect of multiple absorption, is significant Chemical Control rate of adsorption step simultaneously.
Material modified Adsorption thermodynamics is tested
Adsorption free energy is calculated by following formula:
Δ Gads=-RTlnKa
Ka is the Langmuir absorption constant at a temperature of certain,；T is malachite green solution temperature, K；R is gas constant, 8.314J/ (mol K).
The adsorption enthalpy of different temperatures and heat of adsorption can be calculated by following formula:
LnKa=Δ Sads/R-Δ Hads/RT
The thermodynamics that malachite green oxalate is adsorbed by the modified old newspaper fiber of table 4
Δ Gads < 0 as shown in Table 4, illustrates that modified old newspaper fiber is endothermic process to malachite green oxalate, and saturated extent of adsorption raises significantly depending on temperature and raises, but after temperature is more than 45 DEG C, saturated extent of adsorption slightly reduces.Δ Hads simultaneously > 0, illustrates that this reaction is heat absorption.Δ Sads > 0 explanation adsorption process is entropy increasing process in solid liquid interface performance, is spontaneous.
Last it is noted that these are only the preferred embodiments of the present invention; it is not limited to the present invention; although the present invention being described in detail with reference to embodiment; for a person skilled in the art; technical scheme described in foregoing embodiments still can be modified by it; or wherein portion of techniques feature is carried out equivalent; but all within the spirit and principles in the present invention; the any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (5)
1. an old newspaper is as the preparation method of the cation solid absorbent of raw material, it is characterised in that its bag
Include following steps:
(1) old newspaper tears to bits, is soaked in water 24 hours, centrifugal after making beating；
(2) deinking is carried out: according to mass percent, pulp density: 8%, sodium sulfite consumption: 4%,
Tune pH value is 6-7, temperature 60～70 DEG C of immersion 75min；
(3) the centrifugal and old newspaper of drying steps (2) gained, carries out secondary deinking: pulp density: 5%, NaOH
Consumption 0.6%, H2O2Consumption 0.9%, temperature 50 C, soaks 60min；
(4) paper pulp after secondary deinking is dried to constant weight at 50 DEG C, puts in exsiccator standby；
(5) weigh secondary de inked pulp, add 1mol/L phosphoric acid solution, stirring reaction 2h under room temperature；
(6) it is dried to exclusion at 50 DEG C after draining liquid, is warming up to 120 DEG C of heating 1.5h；
(7) with deionized water, the product of step (6) gained is washed to neutral；
(8) it is dried to constant weight at 50 DEG C.
A kind of old newspaper is as the preparation side of the cation solid absorbent of raw material
Method, it is characterised in that described old newspaper is torn into the fragment of 2 × 5cm.
A kind of old newspaper is as the preparation side of the cation solid absorbent of raw material
Method, it is characterised in that in step (5), the ratio of described secondary de inked pulp and phosphoric acid solution is
1:5。
4. an old newspaper modified product, it is characterised in that be to prepare in accordance with the method for claim 1
's.
5. the old newspaper modified product described in claim 4 is in the application prepared on water pollutant adsorbent.
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| CN201610223875.7A CN106000331A (en) | 2016-04-11 | 2016-04-11 | Preparation method for cationic solid adsorption agent with old newspapers as raw material, product and application of product |
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| CN201610223875.7A CN106000331A (en) | 2016-04-11 | 2016-04-11 | Preparation method for cationic solid adsorption agent with old newspapers as raw material, product and application of product |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109647338A (en) * | 2019-01-21 | 2019-04-19 | 安徽农业大学 | The preparation method of disregard message paper base charcoal |
| CN110548493A (en) * | 2019-09-29 | 2019-12-10 | 陕西科技大学 | Deinking waste newspaper-based adsorbent modified by imidazole ionic liquid and preparation method thereof |
| CN116371356A (en) * | 2022-12-30 | 2023-07-04 | 华南理工大学 | Surface functionalized wood pulp derived carbon adsorption material and preparation method and application thereof |
Citations (1)
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| CN102151553A (en) * | 2011-03-28 | 2011-08-17 | 沈阳化工大学 | Method for treating printing and dyeing waste water by taking waste newspaper as adsorbent |
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2016
- 2016-04-11 CN CN201610223875.7A patent/CN106000331A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102151553A (en) * | 2011-03-28 | 2011-08-17 | 沈阳化工大学 | Method for treating printing and dyeing waste water by taking waste newspaper as adsorbent |
Non-Patent Citations (3)
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| CHUNG-HSIN WU ET AL.: "Removal of copper by surface-modified celluloses: kinetics, equilibrium, and thermodynamics", 《DESALINATION AND WATER TREATMENT》 * |
| 李文俊等: "废报纸中性亚硫酸钠脱墨工艺条件的探索", 《湖北造纸》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109647338A (en) * | 2019-01-21 | 2019-04-19 | 安徽农业大学 | The preparation method of disregard message paper base charcoal |
| CN110548493A (en) * | 2019-09-29 | 2019-12-10 | 陕西科技大学 | Deinking waste newspaper-based adsorbent modified by imidazole ionic liquid and preparation method thereof |
| CN116371356A (en) * | 2022-12-30 | 2023-07-04 | 华南理工大学 | Surface functionalized wood pulp derived carbon adsorption material and preparation method and application thereof |
| CN116371356B (en) * | 2022-12-30 | 2024-02-09 | 华南理工大学 | Surface functionalized wood pulp derived carbon adsorption material and preparation method and application thereof |
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Application publication date: 20161012 |