CN105944699B - A kind of composite adsorption resin - Google Patents
A kind of composite adsorption resin Download PDFInfo
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- 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
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Abstract
The invention discloses a kind of composite adsorption resins, using adsorbent B LPAS as raw material, raw material is carried out the following processing and is prepared: (1) taking 5g adsorbent B LPAS to be placed in the sodium hydroxide solution that 150-250mL concentration is 0.5-2.0mol/L and is impregnated 1-3 hours at 10 DEG C~40 DEG C, obtain mixing soak；(2) the mixing soak is then heated to 70-100 DEG C of reaction 0.5-2.0h, reaction product is obtained by filtration, with distilled water flushing, be in neutrality until washing efflux；(3) reaction product dry, pulverize at 65 DEG C~75 DEG C, crosses 60-100 mesh and obtains composite adsorption resin.The ratio that can coordinate chelation group and ion-exchange group in modified lignin resin base adsorbent structure by the above processing method, significantly improves the absorption property to heavy metal ion.
Description
Technical field
The invention belongs to adsorbent preparation technical fields, and in particular to a kind of inexpensive, high-performance lignin-base heavy metal
Ion adsorbent.
Background technique
Currently, modified lignin resin is relatively common as adsorbent for heavy metal, but existing method of modifying is mostly low point
Son amount is modified, and product adsorption effect is promoted not significant.Solution Free Radical grafting copolymerization process can introduce greatly in lignin structure
Adsorption group is measured, while improving the relative molecular mass of lignin and improving space structure, significantly improves lignin to heavy metal
The absorption property of ion.
Inventor studies a kind of lignin graft copolymerization compound adsorption resin and preparation method thereof early stage, sees Chinese invention
Patent, ZL 201310278489.4, the absorption resin are common using method acrylamide, maleic anhydride and the chitosan etc.
Modified preparation lignin graft copolymerization compound adsorption resin (hereinafter referred BLPAMA), achieves certain technical effect.But by
The carboxylic group that maleic anhydride modified lignin introduces is weak ion-exchange group, the suction to modified lignin resin to heavy metal ion
Attached performance has certain limitation.
Currently, it is relatively common, but existing wooden for being used as adsorbent for heavy metal using chemical method modified lignin resin
Plain modified product is mostly gel-type adsorbent, and interior microcellular structure is poor, specific surface area is smaller, in practical applications adsorption group benefit
Low with rate, absorption property is poor.
On the basis of the studies above, inventor is again after research and improvement in several years, it is intended to propose a kind of more excellent
Composite adsorption resin, ingredient can be reduced while there is good adsorbent effect, performance is stablized.
Summary of the invention
In view of the deficiencies of the prior art, the present invention is directed to propose a kind of more excellent composite adsorption resin, side of the invention
Method can coordinate in modified lignin resin base adsorbent structure by handling original adsorbent, after processing chelation group with from
The ratio of sub- cation exchange groups significantly improves the absorption property to heavy metal ion, obtains a kind of composite adsorption tree of function admirable
Rouge.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
Raw material is carried out the following processing and is prepared using adsorbent B LPAS as raw material by a kind of composite adsorption resin:
(1) 5g adsorbent B LPAS is taken to be placed in the sodium hydroxide solution that 150-250mL concentration is 0.5-2.0mol/L in 10
DEG C~40 DEG C at impregnate 1-3 hours, obtain mixing soak；
(2) the mixing soak is then heated to 70-100 DEG C of reaction 0.5-2.0h, reaction product is obtained by filtration, used
Distilled water flushing, until washing efflux is in neutrality；
(3) reaction product dry, pulverize at 65 DEG C~75 DEG C, crosses 60-100 mesh and obtains composite adsorption resin
(hereinafter referred BLPAS-S)；
Wherein, the adsorbent B LPAS is total monomer according to acrylamide and 2- acrylamide-2-methyl propane sulfonic
It calculates, formula and its content are as follows:
The mass ratio of acrylamide and 2- acrylamide-2-methyl propane sulfonic be (1-2.8) ︰ 2, sodium lignin sulfonate with
The mass ratio of total monomer be (0.5-2.0) ︰ 10, the mass content of potassium peroxydisulfate are 0.2%-0.5%, the N of total monomer quality,
The mass content of N '-methylene-bisacrylamide is the 0.1%-0.25% of total monomer quality, and bentonitic mass content is total
The 2%-4% of monomer mass.
The room temperature is preferably 15 DEG C~30 DEG C.
Preferred embodiment, the adsorbent B LPAS are total monomer according to acrylamide and 2- acrylamide-2-methyl propane sulfonic
It calculates, formula and its content are as follows:
The mass ratio of acrylamide and 2- acrylamide-2-methyl propane sulfonic is (1-2) ︰ 2, sodium lignin sulfonate and total
The mass ratio of monomer be (0.5-1.0) ︰ 10, the mass content of potassium peroxydisulfate are 0.25%-0.45%, the N of total monomer quality,
The mass content of N '-methylene-bisacrylamide is the 0.15%-0.25% of total monomer quality, and bentonitic mass content is total
The 3% of monomer mass.
Further preferred scheme, the adsorbent B LPAS are prepared by following methods:
1) weigh that quantitative sodium lignin sulfonate is molten and acrylamide is dissolved separately in distilled water by above-mentioned formula, respectively
Obtain lignin sulfonic acid sodium water solution and acrylamide aqueous solution；
2) 2- acrylamide-2-methyl propane sulfonic, bentonite, N, N '-methylene are sequentially added in acrylamide aqueous solution
Base bisacrylamide, stirring are uniformly mixed, and obtain solution A；
3) then solution A is added in lignin sulfonic acid sodium water solution, adjusting pH is 1.0-4.0, adds persulfuric acid
Potassium, sealing, reacts 1.5h-2.5h, then 1.5h-2.5h is reacted at 70 DEG C -80 DEG C, then at 85 DEG C -90 at 60 DEG C -65 DEG C
1.5h-2.5h is reacted at DEG C, is cured 0.5h-2.5h at 90 DEG C -100 DEG C after having reacted, is obtained reaction product；
4) reaction product is cooling, methanol or ethyl alcohol washing by soaking are used after shredding, and are finally done at 65 DEG C~75 DEG C
It is dry, it crushes, crosses 60 mesh~100 meshes, obtain adsorbent B LPAS.
The adsorbent B LPAS is a kind of improved adsorbent, it eliminates two kinds of original main component chitosans
And maleic anhydride, it introduces after the new ingredient 2- acrylamide-2-methyl propane sulfonic of one kind, not only there is lower cost, and
And there is better adsorption effect, and property is more stable.
Compared with prior art, advantage of the invention is as follows:
1, the preparation of composite adsorption resin of the present invention keeps uncharged amide groups hydrolysis generation in BLPAS structure electronegative
Carboxylic acid sodium base makes sulfonic group be changed into sodium sulfonate group, coordinates the ratio of chelating with ion-exchange group, increases lignin three-dimensional space
Between network repulsion, improve water absorption and swelling performance, enable a large amount of activated adoption groups of absorbent interior participate in heavy metal ion suction
It is attached, significantly improve the absorption property to heavy metal ion.
2, composite adsorption resin of the present invention is preferable to hybrid piles adsorption effect, in 2.0mmol/L binary Pb
(NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively 1.225,1.047mmol/g, Pb2+To Cu2+Selectivity
Adsorption coefficient is 2.623.
3, composite adsorption resin preparation of the present invention is simple, easy to operate, easy industrialized production not high to equipment requirement.
Detailed description of the invention
Fig. 1 is the XPS wide range comparison diagram of BLPAS and BLPAS-S.
Specific embodiment
The present invention will be further explained with reference to the examples below.
The preparation of the adsorbent B LPAS:
Embodiment 1
It weighs 4.156g sodium lignin sulfonate and 11.083g acrylamide is dissolved separately in 30mL distilled water.In propylene
22.167g 2- acrylamide-2-methyl propane sulfonic, 1g bentonite, 0.0582g N, N '-methylene are sequentially added in amide solution
Base bisacrylamide, stirring, be uniformly mixed obtain A liquid.A liquid is added in lignin sulfonic acid sodium solution, adjusting pH value of solution is
4.0,0.116g potassium peroxydisulfate is added, is sealed, after 65 DEG C, 75 DEG C, 85 DEG C are respectively reacted 2h, 95 DEG C of curing 0.5h are cooling, shred
Methanol washing by soaking is used afterwards, dry, pulverize in 65-75 DEG C of vacuum oven, is crossed 60-100 mesh and is obtained bentonite/sulfomethylated lignin
Sour sodium-g-acrylamide -2- acrylamide-2-methyl propane sulfonic composite adsorption resin (BLPAS).At room temperature, BLPAS exists
Binary Pb (the NO of 100mL, 2.0mmol/L3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively 0.593,
0.604mmol/g, Pb2+To Cu2+Selective absorption coefficient be 1.265.
Embodiment 2
Operating method is the same as embodiment 1.
Preparation condition is m (sodium lignin sulfonate): m (total monomer)=1.5:10, m (acrylamide): m (2- acrylamide-
2- methyl propane sulfonic acid)=2:2, m (potassium peroxydisulfate)=0.40%, m (N, N '-methylene-bisacrylamide)=0.15%, pH=
When 2.0, gained composite adsorption resin B LPAS is in binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively
0.570,0.487mmol/g, Pb2+To Cu2+Selective absorption coefficient be 1.355.:
Embodiment 3
Operating method is the same as embodiment 1.
Preparation condition is m (sodium lignin sulfonate): m (total monomer)=1.25:10, m (acrylamide): m (2- acryloyl
Amine -2- methyl propane sulfonic acid)=2.5:2, m (potassium peroxydisulfate)=0.35%, m (N, N '-methylene-bisacrylamide)=0.18%,
When pH=1.0, gained composite adsorption resin B LPAS is in binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance point
Not Wei 0.558,0.496mmol/g, Pb2+To Cu2+Selective absorption coefficient be 1.342.
Embodiment 4:
Operating method is the same as embodiment 1.
Preparation condition is m (sodium lignin sulfonate): m (total monomer)=1.25:10, m (acrylamide): m (2- acryloyl
Amine -2- methyl propane sulfonic acid)=1:2, m (potassium peroxydisulfate)=0.35%, m (N, N '-methylene-bisacrylamide)=0.18%, pH
When=2.5, gained composite adsorption resin B LPAS is in binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance difference
For 0.544,0.467mmol/g, Pb2+To Cu2+Selective absorption coefficient be 1.287.
Embodiment 5
Operating method is the same as embodiment 1.
Preparation condition is m (sodium lignin sulfonate): m (total monomer)=1.5:10, m (acrylamide): m (2- acrylamide-
2- methyl propane sulfonic acid)=2.8:2, m (potassium peroxydisulfate)=0.40%, m (N, N '-methylene-bisacrylamide)=0.20%, pH
When=3.0, gained composite adsorption resin B LPAS is in binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance difference
For 0.375,0.363mmol/g, Pb2+To Cu2+Selective absorption coefficient be 1.084.
The preparation of composite adsorption resin B LPAS-S:
Embodiment 6
The sodium hydroxide solution of 200mL 1.85mol/L is configured first, then to take 5g BLPAS to be placed in above-mentioned sodium hydroxide molten
Then 30 DEG C of immersion 2.0h in liquid are heated to 80 ± 2 DEG C of DEG C of reaction 1.75h in constant temperature water bath, reaction product are obtained by filtration,
With a large amount of distilled water flushings, it is in neutrality until washing efflux；Reaction product dry, pulverize at 75 DEG C ± 2 DEG C, cross 60-100
Mesh obtains reaction lignin base weight metal ion adsorbent BLPAS-S.That is: reaction condition are as follows: naoh concentration
1.85mol/L, 80 DEG C of reaction temperature, reaction time 1.75h.Gained BLPAS-S is in 2.0mmol/L binary Pb (NO3)2/Cu
(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively 1.225,1.047mmol/g, Pb2+To Cu2+Selective absorption coefficient
It is 2.623.
Under identical adsorption conditions, BLPAS is to Pb before reacting2+、Cu2+Adsorbance is respectively 0.593,0.604mmol/g, Pb2+
To Cu2+Selective absorption coefficient be 1.265.Than being respectively increased 2.07,1.73,2.07 times before reaction after reaction.
The elemental analysis of table 1 BLPAS and BLPAS-S
N1s track absorption peak significantly reduces after reacting as shown in Figure 1, and Na1s absorption peak significantly increases, and illustrates amide groups
Hydrolysis generates carboxylic acid sodium；As shown in Table 1,5.78% is reduced compared to N element content after reaction, so that adsorption group-in BLPAS-S
CONH2、-COONa、-SO3The ratio of Na is approximately 1:1:1；Swelling ratio of the BLPAS-S in distilled water is after reaction
244.95g/g is 127.29g/g before reaction；Illustrate that the processing method significantly improves the swelling behavior of adsorbent B LPAS, makes to inhale
The attached dose of a large amount of adsorption groups in inside can participate in absorption heavy metal ion, improve the absorption property of adsorbent.
Embodiment 7
Operating method is substantially with embodiment 1, but operating condition variation is as follows:
Soaking conditions are as follows: soaking time 1.5h, 35 DEG C of soaking temperature；
Reaction condition are as follows: naoh concentration 1.25mol/L, 100 DEG C of reaction temperature, reaction time 0.5h；
Drying condition are as follows: 70 DEG C ± 2 DEG C；
Gained BLPAS-S is in 2.0mmol/L binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively
1.516,1.691mmol/g, Pb2+To Cu2+Selective absorption coefficient be 1.527.
Embodiment 8
Soaking conditions are as follows: soaking time 2.0h, 35 DEG C of soaking temperature；
Reaction condition are as follows: naoh concentration 0.5mol/L, 90 DEG C of reaction temperature, reaction time 0.5h；Drying condition are as follows:
65℃±2℃；
Gained BLPAS-S is in 2.0mmol/L binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively
1.231,1.040mmol/g, Pb2+To Cu2+Selective absorption coefficient be 2.227.
Embodiment 9
Operating method is the same as embodiment 1.
Soaking conditions are as follows: soaking time 1.0h, 40 DEG C of soaking temperature；
Reaction condition are as follows: naoh concentration 1.25mol/L, 100 DEG C of reaction temperature, reaction time 2.0h；
Drying condition are as follows: 75 DEG C ± 2 DEG C；
Gained BLPAS-S is in 2.0mmol/L binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively
1.069,0.677mmol/g, Pb2+To Cu2+Selective absorption coefficient be 3.235.
Embodiment 10
Operating method is the same as embodiment 1.
Soaking conditions are as follows: soaking time 1.5h, 40 DEG C of soaking temperature；
Reaction condition are as follows: naoh concentration 1.25mol/L, 70 DEG C of reaction temperature, reaction time 0.5h；Drying condition
Are as follows: 75 DEG C ± 2 DEG C；
Gained BLPAS-S is in 2.0mmol/L binary Pb (NO3)2/Cu(NO3)2To Pb in solution2+、Cu2+Adsorbance is respectively
1.109,0.781mmol/g, Pb2+To Cu2+Selective absorption coefficient be 2.877.
Claims (2)
1. a kind of composite adsorption resin, characterized in that using adsorbent B LPAS as raw material, raw material is carried out the following processing and is prepared into
It arrives:
(1) take 5g adsorbent B LPAS be placed in 150-250mL concentration be 0.5-2.0mol/L sodium hydroxide solution in 10 DEG C~
It is impregnated 1-3 hours at 40 DEG C, obtains mixing soak；
(2) the mixing soak is then heated to 70-100 DEG C of reaction 0.5-2.0h, reaction product is obtained by filtration, with distillation
Water rinses, until washing efflux is in neutrality；
(3) reaction product dry, pulverize at 65 DEG C~75 DEG C, crosses 60-100 mesh and obtains composite adsorption resin；Institute
Stating composite adsorption resin is Heavy metal ion adsorption resin, and the heavy metal ion is Pb2+；
Wherein, the adsorbent B LPAS is total monomer calculating according to acrylamide and 2- acrylamide-2-methyl propane sulfonic, is matched
Side and its content are as follows:
The mass ratio of acrylamide and 2- acrylamide-2-methyl propane sulfonic is (1-2) ︰ 2, sodium lignin sulfonate and total monomer
Mass ratio be that (0.5-1.0) ︰ 10, the mass content of potassium peroxydisulfate are the 0.25%-0.45%, N, N of total monomer quality '-
The mass content of methylene-bisacrylamide is the 0.15%-0.25% of total monomer quality, and bentonitic mass content is total single
The 3% of weight.
2. composite adsorption resin according to claim 1, characterized in that the adsorbent B LPAS is prepared by following methods
It arrives:
1) weigh that quantitative sodium lignin sulfonate is molten and acrylamide is dissolved separately in distilled water by above-mentioned formula, respectively it is wooden
Quality sulfonic acid sodium water solution and acrylamide aqueous solution；
2) 2- acrylamide-2-methyl propane sulfonic, bentonite, N, N '-di-2-ethylhexylphosphine oxide are sequentially added in acrylamide aqueous solution
Acrylamide, stirring are uniformly mixed, and obtain solution A；
3) then solution A is added in lignin sulfonic acid sodium water solution, adjusting pH is 2.5, adds potassium peroxydisulfate, it seals,
1.5h-2.5h is reacted at 60 DEG C -65 DEG C, then reacts 1.5h-2.5h at 70 DEG C -80 DEG C, is then reacted at 85 DEG C -90 DEG C
1.5h-2.5h cures 0.5h-2.5h at 90 DEG C -100 DEG C after having reacted, obtains reaction product；
4) reaction product is cooling, methanol or ethyl alcohol washing by soaking are used after shredding, finally dry at 65 DEG C~75 DEG C, powder
It is broken, 60 mesh~100 meshes are crossed, adsorbent B LPAS is obtained.
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| CN102675540A (en) * | 2011-03-15 | 2012-09-19 | 中南林业科技大学 | Heavy metal ion adsorption resin and preparation method thereof |
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