CN105617998A - Preparing method for modified chitosan adsorbent - Google Patents
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- CN105617998A CN105617998A CN201511008932.1A CN201511008932A CN105617998A CN 105617998 A CN105617998 A CN 105617998A CN 201511008932 A CN201511008932 A CN 201511008932A CN 105617998 A CN105617998 A CN 105617998A
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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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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention relates to a preparing method for a modified chitosan adsorbent. The invention further relates to application of the modified chitosan adsorbent prepared through the method in treating heavy metal ion wastewater.
Description
Technical field
The invention belongs to water-treatment technology field, it relates to the preparation method of a kind of modified chitosan sorbent material. The present invention also relates to the method adopting obtained modified chitosan sorbent treatment effluent containing heavy metal ions.
Background technology
Derived energy chemical trade effluent component is complicated, usually containing comprising the heavy metal ion such as copper, cobalt, manganese, and other organic macromolecule, suspended substances etc. Existing method of wastewater treatment, such as neutralisation, reduction method, membrane filter method, sulfuration method etc., faces that single treatment amount is little, long processing period, process less effective, processing cost are high, there is the difficult problems such as secondary pollution.
For problems such as effluent containing heavy metal ions complex treatment process, process cost and material cost in derived energy chemical industry are relatively high, this area urgently needs to develop the method for a kind of simple to operate, environmental friendliness, process effluent containing heavy metal ions with low cost.
Summary of the invention
For problems such as effluent containing heavy metal ions complex treatment process, process cost and material cost in derived energy chemical industry are relatively high, the present invention provides a kind of method adopting modified chitosan sorbent treatment effluent containing heavy metal ions. The method has the features such as modified effect is obvious, simple to operate, sorbent material good stability, absorption property significantly improve, thus solves problems of the prior art.
The present invention provides the preparation method of a kind of modified chitosan sorbent material, and the method comprises the following steps:
The preparation of (i) chitosan microlayer model: respectively disperse phase and the focused flow that communicates continuously are declined in fluidic chip, obtained chitosan microlayer model, wherein, described disperse phase comprises the chitosan of 0.5-2 weight part and the aqueous solution of the Glacial acetic acid of 1-2 weight part; The described octane solution comprising the class of department 80 containing 1-2 weight part continuously mutually;
(ii) chitosan microlayer model is crosslinked: is imported in the water-bath solid solution containing glutaraldehyde cross-linking agent by the chitosan microlayer model obtained in step (i), and reacts under slow stirring, cross-linked chitosan microlayer model;
(iii) the crosslinked chitosan microlayer model obtained in step (ii) is transferred in the reception phase solution comprising n-Octanol and octane standing, obtain chitosan microball particle;
(iv) the chitosan microball particle obtained is cleaned in step (iii);
The chitosan microball particle obtained in (v) baking step (iv);
(vi) the chitosan microball particle obtained in step (v) is immersed in butanol solution;
(vii) in the butanol solution immersed with chitosan microball particle in step (vi), epoxy chloropropane is added, and stirring in water bath;
(viii) carry out after completely until the reaction in step (vii), by chitosan microball transfer of granules in polyethyleneimine amine aqueous solution, and the reaction when constantly heating up and slowly stir; And
(ix) the chitosan microball particle obtained in step (viii) is cleaned, and dry and obtain modified chitosan sorbent material.
In one preferred embodiment, in step (i), it may also be useful to disperse phase and the focused flow that communicates continuously are declined in fluidic chip by 1 single passage syringe pump and 1 two channels syringe pump respectively; The viscosity of described chitosan is 200mPa S; The velocity ratio regulating described disperse phase and continuous phase is 1:5-1:10, after the stable generation of chitosan microlayer model, collects chitosan microlayer model.
Another preferred embodiment in, in step (ii), described water-bath solid solution comprises the octane solution of the class of department 80 of the glutaraldehyde containing 0.5-1 weight part and 1-2 weight part; Slow stirring reaction 30-60 minute under the water bath condition of 30-40 DEG C.
Another preferred embodiment in, in step (iii), described reception phase solution comprises the octane solution of 5-8 weight % n-Octanol; Time of repose is 6-8 hour.
Another preferred embodiment in, in step (iv), successively with 50 weight % ethanolic solns and washed with de-ionized water chitosan microball particle 3-4 time.
Another preferred embodiment in, in step (v), vacuum drying temperature is 50-60 DEG C, and drying time is no less than 6 hours.
Another preferred embodiment in, in step (vi), described butanol solution is obtained with 1:1-1:2 dilution by propyl carbinol and deionized water; Chitosan microball particle wherein soak time be 20-30 minute.
Another preferred embodiment in, in step (vii), the addition of described epoxy chloropropane is 0.3-0.5 weight %; Slowly stir 2-3 hour under the water bath condition of 45-50 DEG C.
Another preferred embodiment in, in step (viii), the addition of described polymine is 0.5-1 weight %; Slowly stirring when temperature is no more than 60 DEG C, the reaction times is not less than 3 hours.
Another preferred embodiment in, in step (ix), use successively 50 weight % ethanolic solns and deionized water chitosan microball particle is carried out clean 3-4 time; Bake out temperature is 40-50 DEG C, and drying time is no less than 10 hours.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of the modified chitosan sorbent material according to an embodiment of the invention.
Fig. 2 is the pictorial diagram contrast of the chitosan absorbent according to an embodiment of the invention and modified chitosan sorbent material.
Embodiment
Term
Term chitosan (Chitosan) used herein, refers to the product of chitin deacetylase base. It is the unique natural alkalescence glycosaminoglycan of nature, has good biocompatibility, biological degradability and after product nontoxicity of degrading. Containing a large amount of hydroxyls and amino on its macromolecular chain, wherein amino can react with metal ion, forms metallo-chelate, thus adsorbing metal ions, hydroxyl and amino can also be utilized to be modified by chitosan itself simultaneously, and then strengthen it to metal biosorption performance.
Term focused flow used herein declines Flow Control, and the shearing action between referring to by immiscible fluid prepares dispersant liquid drop, and the microflow control technique as products such as Template preparation particle, gels. Drop microflow control technique can be applicable to multiple crossing domain. In chemical analysis, each drop is an independent enclosed space, enhances the freedom from jamming of sample in drop, not easily causes crossed contamination between sample, it is to increase analysis efficiency is with repeatable; In reaction, significantly promote size uniformity degree and the structure complexity of microreactor, expand microreactor preparation method; In material field, its can be particle, gel, micro-capsule preparation excellent template is provided, give the physical and chemical performance that it is good.
Term microlayer model used herein, refer to a kind of technology manipulating very low volume fluids grown up on micro-fluidic chip in recent years, its principle is: by two kinds of immiscible liquid, taking one wherein as continuous phase, another kind is disperse phase, entering chip by different entrance respectively with disperse phase mutually continuously, in microchannel, disperse phase is cut into the uniform microlayer model of particle diameter of series of discrete continuously mutually under the effect of shearing force. Being wrapped up mutually continuously of each drop independence, forms a closed system with extraneous without exchange of substance, therefore as a microreactor, can complete one group of chemistry or biological respinse, and stable reaction conditions, reliable results.
Present inventor finds after extensive and deep research, absorption method utilizes sorbent material that is natural or synthetic, heavy metal ions in wastewater is carried out physics and chemistry absorption, does not only produce secondary pollution, and there is the performance of recyclable recycling; For problems such as effluent containing heavy metal ions complex treatment process, process cost and material cost in derived energy chemical industry are relatively high, adopt modified chitosan sorbent treatment effluent containing heavy metal ions, wherein with glutaraldehyde as cross linker, the chitosan microball utilizing polymine to be prepared by microflow control technique carries out modification and prepares adsorbent for heavy metal; Compared with tradition sorbent material, divalent heavy metal ions is had very strong absorption property by this sorbent material, particularly cobalt ion is had adsorption selectivity. Based on above-mentioned discovery, the present invention is accomplished.
In a first aspect of the present invention, it provides the preparation method of a kind of modified chitosan sorbent material, the method comprises the following steps:
Step one: the preparation of chitosan microlayer model: the disperse phase of certain component and enter focused flow by single passage syringe pump and two channels syringe pump pump respectively mutually continuously and decline in fluidic chip, obtained chitosan microlayer model;
Step 2: being cross-linked of chitosan microlayer model: the chitosan microlayer model obtained in step one is transferred in the water-bath solid solution containing certain density glutaraldehyde cross-linking agent, reacts for some time under slow agitation condition, make chitosan microlayer model full cross-linked;
Step 3: the chitosan droplet transfer after crosslinked is left standstill a few hours in the reception phase solution being mixed with by a certain percentage by n-Octanol and octane;
Step 4: utilize the chitosan microball several obtained in certain density ethanolic soln and washed with de-ionized water step 3;
Step 5: the chitosan microball vacuum drying a few hours that will obtain in step, solidify completely to chitosan particle;
Step 6: the chitosan particle obtained in step 5 is immersed in certain density butanol solution a few hours;
Step 7: add a certain amount of epoxy chloropropane in the above-mentioned butanol solution immersed with chitosan particle, control bath temperature, slowly stirs, stoichiometric number hour;
Step 8: above-mentioned chitosan particle is transferred in certain density polyethyleneimine amine aqueous solution, and constantly heating up and stoichiometric number hour when slowly stirring;
Step 9: utilize certain density ethanolic soln and deionized water repeatedly to be cleaned by the chitosan particle obtained in step 8 successively, obtain modified chitosan sorbent material after oven dry.
In the present invention, the disperse phase described in step one comprises the aqueous solution of the Glacial acetic acid of chitosan (low viscosity, 200mPa S) that component is about 0.5-2 weight part and about 1-2 weight part; Described comprise the octane solution that component is the class of department 80 containing 1-2 weight part of having an appointment mutually continuously; The velocity ratio controlling described disperse phase and continuous phase is about 1:5-1:10, it is preferable that be about 1:5, after the stable generation of chitosan microlayer model, collects chitosan microlayer model.
In the present invention, the water-bath solid solution described in step 2 comprises the octane solution that component is the class of department 80 adding the have an appointment glutaraldehyde of 0.5-1 weight part and about 1-2 weight part; The chitosan microlayer model obtained in step one is transferred in water-bath solid solution, is being about 30-40 DEG C, it is preferable that slowly stirring under being about the water bath condition of 40 DEG C, the reaction times is about 30-60 minute, it is preferable that be about 1 hour.
In the present invention, the reception phase solution described in step 3 comprises the octane solution of about 5-8 weight % n-Octanol, leaves standstill about 6-8 hour.
In the present invention, in step 4, rinse chitosan microball 3-4 time respectively with about 50 weight % ethanolic solns and deionized water.
In the present invention, the vacuum drying temperature described in step 5 is about 50-60 DEG C, it is preferable that be about 60 DEG C, is no less than 6 hours time of drying.
In the present invention, in step 6, soak chitosan particle with about 50 weight % butanol solutions and it is about 20-30 minute, it is preferable that about 30 minutes.
In the present invention, the addition of the epoxy chloropropane described in step 7 is about 0.3-0.5 weight %, it is preferable that be about 0.5 weight %, at 45-50 DEG C, it is preferable that slowly stir 2-3 hour under the water bath condition of about 50 DEG C.
In the present invention, the addition of the polymine described in step 8 is about 0.5-1 weight %, it is preferable that be about 0.5 weight %, slowly stirs in (temperature is no more than 60 DEG C) when of constantly heating up, and the reaction times is not less than 3 hours.
In the present invention, in step 9, clean in step 8 the chitosan particle that obtains with 50% ethanolic soln 3-4 time; Bake out temperature 40-50 DEG C, it is preferable that be about 40 DEG C, is no less than 10 hours time of drying.
Below referring to accompanying drawing.
Fig. 1 is the preparation flow figure of the modified chitosan sorbent material according to an embodiment of the invention. As shown in Figure 1,1 single passage syringe pump 1 and 1 two channels syringe pump 2 is utilized to decline in fluidic chip 3 by disperse phase and the focused flow that communicates continuously respectively, obtained chitosan microlayer model; The chitosan microlayer model of gained is imported in water-bath solid solution 4, and carries out crosslinking reaction, cross-linked chitosan microlayer model; Chitosan particle after crosslinked is transferred in reception phase solution 5 standing; The chitosan particle of gained is cleaned, dries; The chitosan particle of gained is immersed in butanol solution 6, and adds epoxy chloropropane to this immersed with in the butanol solution of chitosan particle; Chitosan particle is transferred in polyethyleneimine amine aqueous solution 7, and react; Obtain modified chitosan sorbent material 8.
Fig. 2 is the pictorial diagram contrast of the chitosan absorbent according to an embodiment of the invention and modified chitosan sorbent material. As shown in Figure 2, chitosan absorbent (Fig. 2 is right) is reddish-brown microballoon before modified, and the chitosan absorbent (Fig. 2 left) modified through polymine turns into black from reddish-brown.
The major advantage of the present invention is:
The present invention proposes a kind of method adopting modified chitosan sorbent treatment effluent containing heavy metal ions, the method adopts glutaraldehyde as cross linker, and the chitosan microball utilizing polymine to be prepared by microflow control technique carries out modification. Compared with tradition sorbent material, the sorbent material prepared by the present invention not only has uniform grain size and good physical strength, divalent heavy metal ions has very strong absorption property especially, particularly cobalt ion is had adsorption selectivity. The method of the process effluent containing heavy metal ions of the present invention, simple to operate, environmental friendliness, with low cost, waste water can be processed efficiently in conjunction with separating device and reclaim wherein heavy metal, there is the application prospect of industrialization.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment. However, it should be understood that, these embodiments only do not form limitation of the scope of the invention for illustration of the present invention. The test method of unreceipted concrete condition in the following example, usually conveniently condition, or according to the condition that manufacturer advises. Unless otherwise explanation, all per-cent and part number are be weight.
Embodiment 1: utilize the cobalt ion in modified chitosan adsorbent cobalt chloride solution
The preparation of modified chitosan sorbent material:
Step one: by the chitosan aqueous solution of the chitosan (viscosity is 200mPa S) of 2 weight parts and the Glacial acetic acid configuration of 1.5 weight parts as disperse phase, using be added with the class of department 80 (purchased from Chemical Reagent Co., Ltd., Sinopharm Group) of 2 weight parts octane solution as continuous phase; By single passage syringe pump and two channels syringe pump, disperse phase and the focused flow that communicates continuously are declined in fluidic chip, the obtained uniform chitosan microlayer model of particle diameter;
Step 2: the chitosan particle obtained in step one is passed in water-bath solid solution (the octane solution of the glutaraldehyde of 0.7 weight part and the class of department 80 of 2 weight parts), under the water bath condition of 40 DEG C, slowly stir, react 1 hour so that chitosan drop is full cross-linked;
Step 3: by the chitosan droplet transfer after crosslinked to, in the octane solution of 5-8 weight part n-Octanol, leaving standstill 6-8 hour;
Step 4: utilize 50% ethanolic soln of dilution and deionized water to clean the chitosan microball that obtains in step 3 respectively 3-4 time successively;
Step 5: chitosan particle vacuum drying 8 hours under 60 DEG C of conditions that will obtain in step 4, solidifies completely to chitosan particle;
Step 6: the chitosan particle obtained in step 5 is immersed in 50 weight % butanol solutions 30 minutes;
Step 7: the epoxy chloropropane adding 50 weight % in the butanol solution of step 6, slowly stirs 2 hours under the water bath condition of 50 DEG C;
Step 8: the chitosan particle obtained in step 7 is transferred in the polyethyleneimine amine aqueous solution of 0.5 weight %, slowly stir when intensification, for guaranteeing to react completely, the reaction times is 4 hours;
Step 9: utilize 50 weight % ethanolic solns and deionized water repeatedly to be rinsed by the chitosan particle obtained in step 8 successively, dries under 40 DEG C of temperature condition and obtains modified chitosan sorbent material, and drying time is 10 hours.
The absorption of the cobalt ion in cobalt chloride solution:
Take the obtained modified chitosan sorbent material of 0.3g to add in the cobalt chloride solution that 200mL initial pH value is 5, concentration of cobalt ions is 400ppm. Every 1 hour, get the cobalt chloride solution of 1mL, utilize ICP plasma light spectrometer (Agilent science and technology (China) company limited) it to be measured. Finally record modified chitosan sorbent material and reached adsorption equilibrium after 90 hours, be 69.2mg/g to the maximal absorptive capacity of cobalt ion.
Experimental result:
Experiment proves, cobalt ion is had good absorption property by the chitosan absorbent of the present invention.
Embodiment 2: utilize the cupric ion in modified chitosan adsorbent copper-bath
The preparation of modified chitosan sorbent material:
By the obtained modified chitosan sorbent material of method described in embodiment 1.
The absorption of the cupric ion in copper-bath:
Take the obtained modified chitosan sorbent material of 0.3g to add in the copper-bath that 200mL initial pH value is 5, copper ion concentration is 400ppm. Every 1 hour, get the copper-bath of 1mL, utilize ICP plasma light spectrometer it to be measured. Finally record modified chitosan sorbent material and reached adsorption equilibrium after 79 hours, be 74mg/g to the maximal absorptive capacity of cupric ion.
Experimental result:
Experiment proves, cupric ion is had good absorption property by the chitosan absorbent of the present invention.
Embodiment 3: utilize the cobalt in modified chitosan sorbent material selective adsorption copper sulfate and cobalt chloride mixing solutions
Ion
The preparation of modified chitosan sorbent material:
By the obtained modified chitosan sorbent material of method described in embodiment 1.
The selective adsorption of the cobalt ion in copper sulfate and cobalt chloride mixing solutions:
Take that 0.3g modified chitosan sorbent material adds that 200mL initial pH value is 5 to, in copper sulfate that cobalt ion and copper ion concentration are 400ppm and cobalt chloride mixing solutions. Every 1 hour, get the mixing solutions of 1mL, utilize ICP plasma light spectrometer it to be measured. Finally record modified chitosan sorbent material and reached adsorption equilibrium after 87 hours, be 56.3mg/g to the maximal absorptive capacity of cupric ion, be 17.4mg/g to the maximal absorptive capacity of cobalt ion.
Experimental result:
Experiment proves, cupric ion is had good adsorption selectivity by the chitosan absorbent of the present invention.
Above-mentioned listed embodiment is only the better embodiment of the present invention, is not used for limiting the practical range of the present invention. Namely all equivalences done according to the content of the present patent application patent scope change and modify, and all should be the technology category of the present invention.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document. In addition it will be understood that after the above-mentioned teachings having read the present invention, the present invention can be made various changes or modifications by those skilled in the art, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. a preparation method for modified chitosan sorbent material, the method comprises the following steps:
The preparation of (i) chitosan microlayer model: respectively disperse phase and the focused flow that communicates continuously are declined in fluidic chip, obtained chitosan microlayer model, wherein, described disperse phase comprises the chitosan of 0.5-2 weight part and the aqueous solution of the Glacial acetic acid of 1-2 weight part; The described octane solution comprising the class of department 80 containing 1-2 weight part continuously mutually;
(ii) chitosan microlayer model is crosslinked: is imported in the water-bath solid solution containing glutaraldehyde cross-linking agent by the chitosan microlayer model obtained in step (i), and reacts under slow stirring, cross-linked chitosan microlayer model;
(iii) the crosslinked chitosan microlayer model obtained in step (ii) is transferred in the reception phase solution comprising n-Octanol and octane standing, obtain chitosan microball particle;
(iv) the chitosan microball particle obtained is cleaned in step (iii);
The chitosan microball particle obtained in (v) baking step (iv);
(vi) the chitosan microball particle obtained in step (v) is immersed in butanol solution;
(vii) in the butanol solution immersed with chitosan microball particle in step (vi), epoxy chloropropane is added, and stirring in water bath;
(viii) carry out after completely until the reaction in step (vii), by chitosan microball transfer of granules in polyethyleneimine amine aqueous solution, and the reaction when constantly heating up and slowly stir; And
(ix) the chitosan microball particle obtained in step (viii) is cleaned, and dry and obtain modified chitosan sorbent material.
2. the method for claim 1, it is characterised in that, in step (i), it may also be useful to disperse phase and the focused flow that communicates continuously are declined in fluidic chip by 1 single passage syringe pump and 1 two channels syringe pump respectively; The viscosity of described chitosan is 200mPa S; The velocity ratio regulating described disperse phase and continuous phase is 1:5-1:10, after the stable generation of chitosan microlayer model, collects chitosan microlayer model.
3. the method for claim 1, it is characterised in that, in step (ii), described water-bath solid solution comprises the octane solution of the class of department 80 of the glutaraldehyde containing 0.5-1 weight part and 1-2 weight part; Slow stirring reaction 30-60 minute under the water bath condition of 30-40 DEG C.
4. the method for claim 1, it is characterised in that, in step (iii), described reception phase solution comprises the octane solution of 5-8 weight % n-Octanol; Time of repose is 6-8 hour.
5. the method for claim 1, it is characterised in that, in step (iv), successively with 50 weight % ethanolic solns and washed with de-ionized water chitosan microball particle 3-4 time.
6. the method for claim 1, it is characterised in that, in step (v), vacuum drying temperature is 50-60 DEG C, and drying time is no less than 6 hours.
7. the method for claim 1, it is characterised in that, in step (vi), described butanol solution is obtained with 1:1-1:2 dilution by propyl carbinol and deionized water; Chitosan microball particle wherein soak time be 20-30 minute.
8. the method for claim 1, it is characterised in that, in step (vii), the addition of described epoxy chloropropane is 0.3-0.5 weight %; Slowly stir 2-3 hour under the water bath condition of 45-50 DEG C.
9. the method for claim 1, it is characterised in that, in step (viii), the addition of described polymine is 0.5-1 weight %; Slowly stirring when temperature is no more than 60 DEG C, the reaction times is not less than 3 hours.
10. the method for claim 1, it is characterised in that, in step (ix), use 50 weight % ethanolic solns and deionized water to carry out chitosan microball particle cleaning 3-4 time successively; Bake out temperature is 40-50 DEG C, and drying time is no less than 10 hours.
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CN107952416A (en) * | 2017-11-23 | 2018-04-24 | 浙江海洋大学 | A kind of oyster shell whiting chitosan compound microsphere for adsorbing heavy metal and preparation method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106633118A (en) * | 2016-11-10 | 2017-05-10 | 广西大学 | Preparation method of lignin microspheres prepared via mercapto group functionalization |
CN106633118B (en) * | 2016-11-10 | 2019-03-26 | 广西大学 | A kind of preparation method of mercapto-functionalized lignin microballoon |
CN107028052A (en) * | 2017-02-24 | 2017-08-11 | 黄秋丽 | A kind of technique of chitosan microball Clarification of Pineapple Juice |
CN107952416A (en) * | 2017-11-23 | 2018-04-24 | 浙江海洋大学 | A kind of oyster shell whiting chitosan compound microsphere for adsorbing heavy metal and preparation method thereof |
CN107952416B (en) * | 2017-11-23 | 2021-04-23 | 浙江海洋大学 | Shell powder chitosan composite microsphere for adsorbing heavy metals and preparation method thereof |
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