CN107486160A - A kind of nano-cellulose/composite diatomite sorbing material and preparation method thereof - Google Patents

A kind of nano-cellulose/composite diatomite sorbing material and preparation method thereof Download PDF

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Publication number
CN107486160A
CN107486160A CN201710684012.4A CN201710684012A CN107486160A CN 107486160 A CN107486160 A CN 107486160A CN 201710684012 A CN201710684012 A CN 201710684012A CN 107486160 A CN107486160 A CN 107486160A
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nano
cellulose
diatomite
composite
sorbing material
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梁虎南
胡潇
饶泽通
李鹤
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Northeast Electric Power University
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Northeast Dianli University
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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
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14—Diatomaceous earth
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • 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
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • 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
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents

Abstract

A kind of nano-cellulose/composite diatomite sorbing material of the present invention and preparation method thereof, is characterized in：Comprise the following steps：Diatomite is added drop-wise in nano-cellulose suspension；It is 5~9 that pH value is adjusted after stirring；Stir at a certain temperature, obtain nano-cellulose/diatomite mixed solution；Centrifuge washing to neutrality, drying obtains nano-cellulose/diatomite composition；Gained nano-cellulose/diatomite composition is fully dispersed into suspension, and nitrogen protection is lower to add six water and iron chloride and seven water and ferrous sulfate, heating stirring reaction, centrifuge washing, vacuum drying, obtains magnetic Nano cellulose/composite diatomite sorbing material.Preparation technology of the present invention is simple, reaction condition is gentle, made nano-cellulose/composite diatomite sorbing material and magnetic Nano cellulose/composite diatomite sorbing material specific surface area are big, advantages of good adsorption effect, and magnetic Nano cellulose/composite diatomite sorbing material is good to heavy metal ion in water and organic dyestuff removal effect.

Description

A kind of nano-cellulose/composite diatomite sorbing material and preparation method thereof
Technical field
The invention belongs to chemical material technical field, and in particular to sorbing material, be a kind of nano-cellulose/tripolite compound Close sorbing material and preparation method thereof.
Background technology
Adsorption process is that solid absorbent utilizes its own face active group, concrete dynamic modulus, high-specific surface area, is inhaled by physics Attached, chemisorbed, physical and chemical adsorption, ion exchange etc. are reacted, and realize has to the heavy metal ion in liquid, organic dyestuff etc. The process of evil pollutant removal.
Nano-cellulose is the cellulose for having nano-scale, is a kind of natural polymer organic matter, have source it is wide, into This low, environment-friendly, biochemical activity and biodegradability, great amount of hydroxy group be present in nano-cellulose, generation can be passed through The reactions such as esterification, etherificate and other materials are compound.Diatomite is to be formed by the shell wall of Diatomeae unicellular lower eukaryote after diagenesis, With high porosity and high-ratio surface, it is SiO that it, which is mainly formed,2, intramolecular contains silicone hydroxyl, have preferable chemism and Stronger adsorption capacity.Nano-cellulose and diatomite all have higher as relatively conventional sorbing material constituent Specific surface area, surface-active and mechanical strength, there is relatively broad answer in Adsorption heavy metal ion and organic dyestuff field With.
The current report about nano-cellulose and composite diatomite is not yet reported in media.
The content of the invention
The technical problems to be solved by the invention are：A kind of the shortcomings that overcoming prior art, there is provided nano-cellulose/diatom Native composite adsorbing material and preparation method thereof, to assign nano-cellulose/diatomite more comprehensive absorption property, extension adsorption material The application of material.
The present invention solve technical problem scheme be：A kind of preparation side of nano-cellulose/composite diatomite sorbing material Method, it is characterized in that：It comprises the following steps：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
(2) after the first mixed solution being stirred into 5~10min, the pH value of the first mixed solution of regulation is 5~9；
(3) the first mixed solution (2) step obtained stirs 2~6h at a temperature of 40~80 DEG C, obtains nano-cellulose/silicon Diatomaceous earth mixed solution；
(4) centrifuge washing nano-cellulose/diatomite mixed solution to neutrality, is dried to constant weight, that is, obtains nano-cellulose/silicon Diatomaceous earth compound.
The nano-cellulose is 2 with diatomaceous mass ratio:1~3:2.
The step (1) in, the preparation method of nano-cellulose suspension is：
By nano-cellulose using solid-to-liquid ratio as 1000:1~5 is added to the water；Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasound Ripple crusher 25~35min of Ultrasonic Pulverization under 1200W power, obtains nano-cellulose solution.
The step (2) in, the pH value of the first mixed solution is adjusted using sulfuric acid solution or sodium hydroxide solution.
The step (4) in, its centrifuge washing is：At a temperature of 20~30 DEG C, with 10 × 103~14 × 103Rpm's turns Fast centrifuge washing, each centrifuge washing time are 3~8min, centrifuge washing 4~5 times.
The step (4) in, drying temperature be 100 DEG C.
A kind of nano-cellulose/composite diatomite sorbing material, it is characterized in that：Pass through a kind of nano-cellulose/diatomite The product that the preparation method of composite adsorbing material obtains.
A kind of method that magnetic Nano composite adsorbing material is prepared with nano-cellulose/composite diatomite sorbing material, its It is characterized in：Comprise the following steps：
(1) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (1)；
(2) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (2)；
(3) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (3)；
(4) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (4)；
By nano-cellulose/diatomite composition in water it is fully dispersed after, be slowly added to six water and chlorine in a nitrogen environment Change iron and seven water and ferrous sulfate, 30~40min is stirred at a temperature of 60~70 DEG C and obtains the first turbid solution, regulation first is muddy Turbid pH value reaches 11~12, continues 1~2h of stirring, obtains magnetic Nano cellulose/diatomite turbid solution；
In the magnetic Nano cellulose/diatomite turbid solution, the mass ratio of nano-cellulose/diatomite and magnetic iron oxide is 2:1~1:2；
Described magnetic iron oxide by six water and iron chloride, seven water and ferrous sulfate reaction generation, six water and iron chloride with The mol ratio of seven water and ferrous sulfate is 1:1；
By step (5) middle gained magnetic Nano cellulose/diatomite turbid solution centrifuge washing to it is neutral, be dried under vacuum to perseverance Weight, obtains magnetic Nano composite adsorbing material.
The step (5) in, with sodium hydroxide solution adjust the first turbid solution pH value.
The step (6) in, its centrifuge washing is：At a temperature of 20~30 DEG C, with 10 × 103~14 × 103Rpm's turns Fast centrifuge washing, each centrifuge washing time are 3~8min, centrifuge washing 8~10 times.
The step (6) in, vacuum drying temperature be 55~60 DEG C.
One kind is with nano-cellulose/magnetic Nano composite adsorbing material made from composite diatomite sorbing material, its feature It is：The production that method by preparing magnetic Nano composite adsorbing material with nano-cellulose/composite diatomite sorbing material obtains Product.
The invention has the advantages that：
（1）The primary raw material of the present invention is nano-cellulose and diatomite, and both inexpensive green material, inhales Without harmful side product when attached, dyestuff and heavy metal ion after absorption can be collected by desorbing, and be truly realized green, can hold Supervention exhibition；
（2）Contain magnetic material in magnetic Nano cellulose/composite diatomite sorbing material prepared by the present invention, in magnetic fields Under, the rapidly and efficiently removal of adsorbent can be realized, reduces large scale equipment demand.
Preparation technology of the present invention is simple, reaction condition is gentle, made nano-cellulose/composite diatomite sorbing material and magnetic Property nano-cellulose/composite diatomite sorbing material specific surface area is big, advantages of good adsorption effect, magnetic Nano cellulose/tripolite compound It is good to heavy metal ion in water and organic dyestuff removal effect to close sorbing material.
The organic dyestuff and heavy metal that magnetic Nano cellulose/composite diatomite sorbing material of the present invention is used in waste water The absorption of ion.
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1, embodiment 1 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 5；
(3) the first mixed solution (2) step obtained stirs 2h at a temperature of 40 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 1 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 1/composite diatomite sorbing material is 35.04 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 16.38 (mg/g).
Embodiment 2, embodiment 2 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 25min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 7；
(3) the first mixed solution (2) step obtained stirs 4h at a temperature of 60 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 1 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 2/composite diatomite sorbing material is 31.12 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 15.93 (mg/g).
Embodiment 3, embodiment 3 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the first mixed solution is adjusted using 0.5mol/L sodium hydroxide solution PH value, make the first mixed solution pH be 9；
(3) the first mixed solution (2) step obtained stirs 6h at a temperature of 80 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 1 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 3/composite diatomite sorbing material is 33.16 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 15.31 (mg/g).
Embodiment 4, embodiment 4 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 35min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the first mixed solution is adjusted using 0.5mol/L sodium hydroxide solution PH value, make the first mixed solution pH be 9；
(3) the first mixed solution (2) step obtained stirs 4h at a temperature of 40 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
In the nano-cellulose/diatomite mixed solution, nano-cellulose is 2 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 4/composite diatomite sorbing material is 24.22 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 14.9 (mg/g).
Embodiment 5, embodiment 5 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 5；
(3) the first mixed solution (2) step obtained stirs 6h at a temperature of 60 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 2 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 5/composite diatomite sorbing material is 27.99 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 13.78 (mg/g).
Embodiment 6, embodiment 6 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 7；
(3) the first mixed solution (2) step obtained stirs 2h at a temperature of 80 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 2 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 6/composite diatomite sorbing material is 25.16 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 10.48 (mg/g).
Embodiment 7, embodiment 7 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 35min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 7；
(3) the first mixed solution (2) step obtained stirs 6h at a temperature of 40 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 3 with diatomaceous mass ratio:2；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 7/composite diatomite sorbing material is 34.89 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 13.2 (mg/g).
Embodiment 8, embodiment 8 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the first mixed solution is adjusted using 0.5mol/L sodium hydroxide solution PH value, make the first mixed solution pH be 9；
(3) the first mixed solution (2) step obtained stirs 2h at a temperature of 60 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 3 with diatomaceous mass ratio:2；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 8/composite diatomite sorbing material is 36.6 (mg/ to MB adsorption capacity G), to Pb2+Adsorption capacity 16.89 (mg/g).
Embodiment 9, embodiment 9 are a kind of nano-cellulose/composite diatomite sorbing materials, and its preparation method includes following Step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 5；
(3) the first mixed solution (2) step obtained stirs 4h at a temperature of 80 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 3 with diatomaceous mass ratio:2；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 9/composite diatomite sorbing material is 27.67 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 10.69 (mg/g).
Embodiment 10, embodiment 10 are a kind of nano-cellulose/composite diatomite sorbing materials, its preparation method include with Lower step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 35min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the first mixed solution is adjusted using 0.5mol/L sodium hydroxide solution PH value, make the first mixed solution pH be 9；
(3) the first mixed solution (2) step obtained stirs 4h at a temperature of 40 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 2 with diatomaceous mass ratio:3；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 10/composite diatomite sorbing material is 36.97 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 16.78 (mg/g).
Embodiment 11, embodiment 11 are a kind of nano-cellulose/composite diatomite sorbing materials, its preparation method include with Lower step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 5；
(3) the first mixed solution (2) step obtained stirs 6h at a temperature of 60 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 2 with diatomaceous mass ratio:3；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 11/composite diatomite sorbing material is 40.3 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 20.98 (mg/g).
Embodiment 12, embodiment 12 are a kind of nano-cellulose/composite diatomite sorbing materials, its preparation method include with Lower step：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 25min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 7；
(3) the first mixed solution (2) step obtained stirs 2h at a temperature of 80 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 2 with diatomaceous mass ratio:3；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition.
After testing, the nano-cellulose of embodiment 12/composite diatomite sorbing material is 38.66 to MB adsorption capacity (mg/g), to Pb2+Adsorption capacity 18.53 (mg/g).
Embodiment 13, embodiment 13 are one kind with nano-cellulose/magnetic Nano made from composite diatomite sorbing material Composite adsorbing material, its preparation method comprise the following steps：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 5；
(3) the first mixed solution (2) step obtained stirs 2h at a temperature of 60 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 1 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition；
By nano-cellulose/diatomite composition in water it is fully dispersed after, be slowly added to six water and chlorine in a nitrogen environment Change iron, seven water and ferrous sulfate, six water and iron chloride and seven water and ferrous sulfate reaction generation magnetic iron oxide, six water with Iron chloride and the mol ratio of seven water and ferrous sulfate are 1:1；30min is stirred at a temperature of 60 DEG C and obtains the first turbid solution, to Sodium hydroxide solution to the first turbid solution pH value that 1mol/L is slowly added dropwise in first turbid solution reaches 11~12, continues to stir 2h, obtain magnetic Nano cellulose/diatomite turbid solution；
In the magnetic Nano cellulose/diatomite turbid solution, the mass ratio of nano-cellulose/diatomite and magnetic iron oxide is 2:1；
(6) at a temperature of 20~30 DEG C, with 10 × 103~14 × 103Rpm rotating speed is by the magnetic Nano of step (5) middle gained Cellulose/diatomite turbid solution 3~8min of centrifuge washing, centrifuge washing 8~10 times is to neutral, and vacuum is done at a temperature of 55~60 DEG C It is dry to constant weight, obtain magnetic Nano composite adsorbing material.
After testing, embodiment 13 with nano-cellulose/compound suction of magnetic Nano made from composite diatomite sorbing material Enclosure material is 51.89 (mg/g) to MB adsorption capacity, to Pb2+Adsorption capacity 26.44 (mg/g).
Embodiment 14, embodiment 14 are one kind with nano-cellulose/magnetic Nano made from composite diatomite sorbing material Composite adsorbing material, its preparation method comprise the following steps：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 5；
(3) the first mixed solution (2) step obtained stirs 2h at a temperature of 60 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 1 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition；
By nano-cellulose/diatomite composition in water it is fully dispersed after, be slowly added to six water and chlorine in a nitrogen environment Change iron, seven water and ferrous sulfate, six water and iron chloride and seven water and ferrous sulfate reaction generation magnetic iron oxide, six water with Iron chloride and the mol ratio of seven water and ferrous sulfate are 1:1；30min is stirred at a temperature of 60 DEG C and obtains the first turbid solution, to Sodium hydroxide solution to the first turbid solution pH value that 1mol/L is slowly added dropwise in first turbid solution reaches 11~12, continues to stir 2h, obtain magnetic Nano cellulose/diatomite turbid solution；
In the magnetic Nano cellulose/diatomite turbid solution, the mass ratio of nano-cellulose/diatomite and magnetic iron oxide is 1:1；
(6) at a temperature of 20~30 DEG C, with 10 × 103~14 × 103Rpm rotating speed is by the magnetic Nano of step (5) middle gained Cellulose/diatomite turbid solution 3~8min of centrifuge washing, centrifuge washing 8~10 times is to neutral, and vacuum is done at a temperature of 55~60 DEG C It is dry to constant weight, obtain magnetic Nano composite adsorbing material.
After testing, embodiment 14 with nano-cellulose/compound suction of magnetic Nano made from composite diatomite sorbing material Enclosure material is 54.29 (mg/g) to MB adsorption capacity, to Pb2+Adsorption capacity 28 (mg/g).
Embodiment 15, embodiment 15 are one kind with nano-cellulose/magnetic Nano made from composite diatomite sorbing material Composite adsorbing material, its preparation method comprise the following steps：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
The preparation method of the nano-cellulose suspension is：By nano-cellulose using solid-to-liquid ratio as 1000:1 is added to the water； Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasonic grind instrument under 1200W power Ultrasonic Pulverization 30min, obtain Nanowire Tie up plain solution；
(2) after the first mixed solution being stirred into 5~10min, the pH of the first mixed solution is adjusted using 0.5mol/L sulfuric acid solution Value, the pH for making the first mixed solution are 5；
(3) the first mixed solution (2) step obtained stirs 2h at a temperature of 60 DEG C, obtains nano-cellulose/diatomite and mixes Close solution；
The nano-cellulose is 1 with diatomaceous mass ratio:1；
(4) at a temperature of 20 DEG C, with 13 × 103Rpm rotating speed centrifuge washing nano-cellulose/diatomite mixed solution, every time The centrifuge washing time is 5min, and centrifuge washing 4~5 times is dried to constant weight at a temperature of 100 DEG C, that is, obtains nanofiber to neutral Element/diatomite composition；
By nano-cellulose/diatomite composition in water it is fully dispersed after, be slowly added to six water and chlorine in a nitrogen environment Change iron, seven water and ferrous sulfate, six water and iron chloride and seven water and ferrous sulfate reaction generation magnetic iron oxide, six water with Iron chloride and the mol ratio of seven water and ferrous sulfate are 1:1；30min is stirred at a temperature of 60 DEG C and obtains the first turbid solution, to Sodium hydroxide solution to the first turbid solution pH value that 1mol/L is slowly added dropwise in first turbid solution reaches 11~12, continues to stir 2h, obtain magnetic Nano cellulose/diatomite turbid solution；
In the magnetic Nano cellulose/diatomite turbid solution, the mass ratio of nano-cellulose/diatomite and magnetic iron oxide is 1:2；
(6) at a temperature of 20~30 DEG C, with 10 × 103~14 × 103Rpm rotating speed is by the magnetic Nano of step (5) middle gained Cellulose/diatomite turbid solution 3~8min of centrifuge washing, centrifuge washing 8~10 times is to neutral, and vacuum is done at a temperature of 55~60 DEG C It is dry to constant weight, obtain magnetic Nano composite adsorbing material.
After testing, embodiment 15 with nano-cellulose/compound suction of magnetic Nano made from composite diatomite sorbing material Enclosure material is 50.13 (mg/g) to MB adsorption capacity, to Pb2+Adsorption capacity 40 (mg/g).
As control, by the nano-cellulose of prior art to MB and Pb2+Adsorption capacity and diatomite to MB sum Pb2+Adsorption capacity detected, the MB is methylene blue.And form nano-cellulose, diatomite and the present invention Embodiment 1~15 is for MB and Pb2+The adsorption capacity table of comparisons, be shown in Table 1：
Table 1
Sequence number Embodiment To MB adsorption capacity (mg/g) To Pb2+Adsorption capacity (mg/g)
1 Nano-cellulose 25.63 11.4
2 Diatomite 21.56 11.65
3 Embodiment 1 35.04 16.38
4 Embodiment 2 31.12 15.93
5 Embodiment 3 33.16 15.31
6 Embodiment 4 24.22 14.9
7 Embodiment 5 27.99 13.78
8 Embodiment 6 25.16 10.48
9 Embodiment 7 34.89 13.2
10 Embodiment 8 36.6 16.89
11 Embodiment 9 27.67 10.69
12 Embodiment 10 36.97 16.78
13 Embodiment 11 40.3 20.98
14 Embodiment 12 38.66 18.53
15 Embodiment 13 51.89 26.44
16 Embodiment 14 54.29 28
17 Embodiment 15 50.13 40
Wherein, embodiment 1~12 is nano-cellulose/composite diatomite sorbing material, and embodiment 13~15 is with nanofiber Element/magnetic Nano composite adsorbing material made from composite diatomite sorbing material.
As shown in Table 1, embodiment 1~12, nano-cellulose/composite diatomite sorbing material are to MB adsorption capacity 24.22~40.3, to Pb2+Adsorption capacity be 10.48-20.98；Embodiment 13~15, with nano-cellulose/tripolite compound It is 50.13~54.29, to Pb to MB adsorption capacity to close magnetic Nano composite adsorbing material made from sorbing material2+Absorption Capacity is 26.44-40；And nano-cellulose is 25.63, to Pb to MB adsorption capacity2+Adsorption capacity be 11.4；Diatom Soil is 21.56, to Pb to MB adsorption capacity2+Adsorption capacity be 11.65.
Therefore, to MB adsorption capacity, its adsorption effect is with nano-cellulose/magnetic made from composite diatomite sorbing material Property nano composite adsorption material ＞ nano-celluloses/composite diatomite sorbing material ＞ nano-cellulose ＞ diatomite, to Pb2+ Adsorption capacity, its adsorption effect is with nano-cellulose/magnetic Nano composite adsorption material made from composite diatomite sorbing material Expect ＞ nano-celluloses/composite diatomite sorbing material ＞ diatomite ＞ nano-celluloses.
In embodiment 1~12, nano-cellulose/composite diatomite sorbing material, held with absorption of the embodiment 11 to MB Amount and Pb2+Adsorption capacity to be optimal, in embodiment 13~15, with made from nano-cellulose/composite diatomite sorbing material In magnetic Nano composite adsorbing material, adsorption capacity and Pb with embodiment 15 to MB2+Adsorption capacity to be optimal.
Above-described embodiment only illustrates the principle and its effect of the present invention, not for the limitation present invention.It is any to be familiar with The personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Therefore, Such as those of ordinary skill in the art without departing from disclosed spirit with being completed under technological thought All equivalent modifications or change, still fall within the present invention claims.

Claims (8)

1. a kind of preparation method of nano-cellulose/composite diatomite sorbing material, it is characterized in that：It comprises the following steps：
By diatomite in water it is fully dispersed after, be added drop-wise in nano-cellulose suspension and obtain the first mixed solution；
(2) after the first mixed solution being stirred into 5~10min, the pH value of the first mixed solution of regulation is 5 ~ 9；
(3) the first mixed solution (2) step obtained stirs 2~6h at a temperature of 40 ~ 80 DEG C, obtains nano-cellulose/silicon Diatomaceous earth mixed solution；
(4) centrifuge washing nano-cellulose/diatomite mixed solution to neutrality, is dried to constant weight, that is, obtains nano-cellulose/silicon Diatomaceous earth compound；
The nano-cellulose is 2 with diatomaceous mass ratio:1~3:2；
A kind of preparation method of nano-cellulose/composite diatomite sorbing material as claimed in claim 1, it is characterized in that：Institute In stating step (1), the preparation method of nano-cellulose suspension is：
By nano-cellulose using solid-to-liquid ratio as 1000:1~5 is added to the water；Stirring is dissolved to abundant at a temperature of 50 DEG C；With ultrasound Ripple crusher 25 ~ 35min of Ultrasonic Pulverization under 1200W power, obtains nano-cellulose solution.
2. a kind of preparation method of nano-cellulose/composite diatomite sorbing material as claimed in claim 1, it is characterized in that： The step (4) in, its centrifuge washing is：At a temperature of 20~30 DEG C, with 10 × 103~14 × 103Rpm rotating speed centrifugation is washed Wash, each centrifuge washing time is 3~8min, centrifuge washing 4 ~ 5 times.
3. a kind of preparation method of nano-cellulose/composite diatomite sorbing material as claimed in claim 1, it is characterized in that： The step (4) in, drying temperature be 100 DEG C.
4. a kind of nano-cellulose/composite diatomite sorbing material, it is characterized in that：The production obtained with claim 1 methods described Product.
5. a kind of method for preparing magnetic Nano composite adsorbing material with nano-cellulose/composite diatomite sorbing material, it is special Sign is：Comprise the following steps：
(1) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (1)；
(2) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (2)；
(3) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (3)；
(4) the preparation method step of same nano-cellulose/composite diatomite sorbing material is (4)；
By nano-cellulose/diatomite composition in water it is fully dispersed after, be slowly added to six water and chlorine in a nitrogen environment Change iron, seven water and ferrous sulfate, 30~40min is stirred at a temperature of 60~70 DEG C and obtains the first turbid solution, regulation first is muddy The pH value of turbid reaches 11 ~ 12, continues 1~2h of stirring, obtains magnetic Nano cellulose/diatomite turbid solution；
In the magnetic Nano cellulose/diatomite turbid solution, the mass ratio of nano-cellulose/diatomite and magnetic iron oxide is 2:1~1:2；
Described magnetic iron oxide by six water and iron chloride, seven water and ferrous sulfate reaction generation, six water and iron chloride with The mol ratio of seven water and ferrous sulfate is 1:1；
By step (5) middle gained magnetic Nano cellulose/diatomite turbid solution centrifuge washing to it is neutral, be dried under vacuum to perseverance Weight, obtains magnetic Nano composite adsorbing material.
6. one kind as claimed in claim 6 prepares the compound suction of magnetic Nano with nano-cellulose/composite diatomite sorbing material The preparation method of enclosure material, it is characterized in that：The step (6) in, its centrifuge washing is：At a temperature of 20~30 DEG C, with 10 × 103~14 × 103Rpm rotating speed centrifuge washing, each centrifuge washing time are 3~8min, centrifuge washing 8 ~ 10 times.
7. one kind as claimed in claim 6 prepares the compound suction of magnetic Nano with nano-cellulose/composite diatomite sorbing material The preparation method of enclosure material, it is characterized in that：The step (6) in, vacuum drying temperature be 55~60 DEG C.
8. it is a kind of with nano-cellulose/magnetic Nano composite adsorbing material made from composite diatomite sorbing material, it is characterized in that： The product obtained with claim 6 methods described.
CN201710684012.4A 2017-08-11 2017-08-11 A kind of nano-cellulose/composite diatomite sorbing material and preparation method thereof Pending CN107486160A (en)

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