CN110124610A - A kind of water body chlorine residue adsorbent and preparation method thereof - Google Patents

A kind of water body chlorine residue adsorbent and preparation method thereof Download PDF

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CN110124610A
CN110124610A CN201910350906.9A CN201910350906A CN110124610A CN 110124610 A CN110124610 A CN 110124610A CN 201910350906 A CN201910350906 A CN 201910350906A CN 110124610 A CN110124610 A CN 110124610A
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chlorine residue
powder
water body
diopside
adsorbent
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CN110124610B (en
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王文静
阳重阳
曹姝文
李锐敬
许嘉辉
刘晓永
周文栋
杨炜雯
黄逸龙
刘诚
钟华东
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GUANGZHOU ENVIRONMENTAL PROTECTION ENGINEERING DESIGNING INST Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14Diatomaceous earth
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of water body chlorine residue adsorbent and preparation method thereof, the preparation method includes the following steps: that S1. takes dry diopside powder and diatomite powder to be uniformly mixed, and obtains mixture;The diopside powder and diatomite powder cross 200 meshes;S2. by the mixture of step S1. in 700~800 DEG C of 100~120min of temperature lower calcination, then natural cooling, obtains precalcining product;S3. the precalcining product of step S2. is obtained into the water body chlorine residue adsorbent in 900~1000 DEG C of 50~70min of temperature lower calcination.The diopside powder and diatomite powder mixture that the present invention used 200 meshes by successively calcining twice, and control the temperature and time of calcining, a kind of water body chlorine residue adsorbent haveing excellent performance successfully is prepared, water body chlorine residue adsorbent, which is made, can be effectively reduced tap water residual chlorine concentration, reduce the mankind and suffers from cancer risk as caused by disinfection by-products, and alkalescent is still kept after a certain amount of chlorine residue of absorption, it is a kind of safe and healthy water body chlorine residue adsorbent.

Description

A kind of water body chlorine residue adsorbent and preparation method thereof
Technical field
The present invention relates to the processing technology fields of tap water, more particularly, to a kind of water body chlorine residue adsorbent and its system Preparation Method.
Background technique
With the improvement of the quality of life, requirement of the people to drinking-water, which also rises to, focuses on healthy and safe level.Tap water Chlorination can guarantee drinking water safety, but in water on the one hand excessive chlorine residue will affect the mouthfeel and smell of water, another party Face can generate disinfection by-products with the natural organic matter reaction in water and threaten human health.At present except chlorine residue research compared with It is few, and removal efficiency is not high, should not promote and apply.In the prior art, activated carbon adsorption chlorine residue, such as Chinese patent are generally used CN201959605U and CN102107994A is all made of active carbon as chlorine residue adsorbent material, but after activated carbon adsorption chlorine residue Understand gradually slant acidity, the bearing structure for carrying adsorbent material may be corroded.
Therefore, a kind of water body chlorine residue adsorbent that can remove chlorine residue in tap water is needed.
Summary of the invention
The present invention is to overcome the defect that chlorine residue removal rate is not high described in the above-mentioned prior art, provides a kind of water body chlorine residue suction Attached dose of preparation method, water body chlorine residue adsorbent obtained can be effectively reduced tap water residual chlorine concentration, reduce the mankind by disappearing Suffer from cancer risk caused by toxic byproduct, and adsorb a certain amount of chlorine residue and still keep alkalescent later, is a kind of safe and healthy Water body chlorine residue adsorbent.
Another object of the present invention is to provide water body chlorine residue adsorbents made from above-mentioned preparation method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of water body chlorine residue adsorbent, includes the following steps:
S1. it takes dry diopside powder and diatomite powder to be uniformly mixed, obtains mixture;The diopside powder and Diatomite powder crosses 200 meshes;
S2. by the mixture of step S1. in 700~800 DEG C of 100~120min of temperature lower calcination, then natural cooling, is obtained To precalcining product;
S3. the precalcining product of step S2. is obtained into the water body in 900~1000 DEG C of 50~70min of temperature lower calcination Chlorine residue adsorbent.
The present invention controls the temperature and time of calcining by successively calcining twice, and it is excellent that a kind of performance is successfully prepared Different water body chlorine residue adsorbent, be made water body chlorine residue adsorbent can be effectively reduced tap water residual chlorine concentration, reduce the mankind by Suffer from cancer risk caused by disinfection by-products, and adsorb a certain amount of chlorine residue and still keep alkalescent later, is a kind of safe and healthy Water body chlorine residue adsorbent.
Calcining for the first time is precalcining, and condition is 700~800 DEG C of 100~120min of temperature lower calcination, then naturally cold But.Carry out second of calcining again, the temperature of second calcining is higher, condition be specially 900~1000 DEG C of temperature lower calcinations 50~ 70min.Inventors have found that the natural cooling between calcining is necessary twice, if will be unable to prepare without natural cooling The water body chlorine residue adsorbent being had excellent performance, it may be possible to carry out second of calcining after natural cooling again and advantageously form and can increase The micro-structure or other substances of strong absorption chlorine residue ability.
Moreover, the partial size of diopside powder and diatomite powder needs to control in suitable range.Partial size is excessive, by nothing The water body chlorine residue adsorbent haveing excellent performance is prepared in method.The aperture of 200 meshes is 75 μm.It needs to control diopside in the present invention The partial size of powder and diatomite powder is less than 75 μm.
In the present invention, calcining is to calcine in air;Muffle furnace calcining specifically can be used.
Preferably, the mass ratio of the diopside powder and diatomite powder is 1: (3~6).Inventor is the study found that thoroughly The mass ratio of pyroxene powder and diatomite powder is 1: when (3~6), the chlorine residue absorption property of water body chlorine residue adsorbent obtained is more It is good.
Preferably, the mass ratio of the diopside powder and diatomite powder is 1: 4.
Preferably, 90 after the diopside powder and diatomite powder of the drying are ground by diopside and diatomite respectively Drying obtains at a temperature of~110 DEG C.The drying is specially dry to constant weight.
Preferably, described grind is carried out by ball mill.
Preferably, the calcining of step S1. and S2. is carried out in Muffle furnace, and the mixture is placed in porcelain crucible.
The present invention protects water body chlorine residue adsorbent made from above-mentioned preparation method simultaneously.
Compared with prior art, the beneficial effects of the present invention are:
The present invention used the diopside powder of 200 meshes and diatomite powder mixture to pass through and successively calcined twice, and The temperature and time for controlling calcining, is successfully prepared a kind of water body chlorine residue adsorbent haveing excellent performance, and water body chlorine residue is made and inhales Attached dose can be effectively reduced tap water residual chlorine concentration, reduces the mankind and suffers from cancer risk as caused by disinfection by-products, and adsorbs Alkalescent is still kept after a certain amount of chlorine residue, is a kind of safe and healthy water body chlorine residue adsorbent.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
Raw material in embodiment can be by being commercially available;
Unless stated otherwise, the present invention uses reagent, method and apparatus for the art conventional reagent, method and are set It is standby.
Embodiment 1
A kind of preparation method of water body chlorine residue adsorbent, the specific steps are as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 4 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 700 DEG C of temperature lower calcinations 100min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 1000 DEG C of temperature lower calcinations 50min, natural cooling obtain water body chlorine residue adsorbent.
Embodiment 2
The present embodiment prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 3 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 800 DEG C of temperature lower calcinations 100min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 900 DEG C of temperature lower calcinations 50min, natural cooling obtain water body chlorine residue adsorbent.
Embodiment 3
The present embodiment prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 5 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 800 DEG C of temperature lower calcinations 120min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 900 DEG C of temperature lower calcinations 70min, natural cooling obtain water body chlorine residue adsorbent.
Embodiment 4
The present embodiment prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 3 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 700 DEG C of temperature lower calcinations 100min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 1000 DEG C of temperature lower calcinations 50min, natural cooling obtain water body chlorine residue adsorbent.
Embodiment 5
The present embodiment prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 6 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 700 DEG C of temperature lower calcinations 100min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 1000 DEG C of temperature lower calcinations 50min, natural cooling obtain water body chlorine residue adsorbent.
Comparative example 1
This comparative example prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 4 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 700 DEG C of temperature lower calcinations 100min;
S3. it after the completion of step S2., without natural cooling, is transferred quickly to have warmed up into 1000 DEG C of Muffle furnace, 1000 DEG C of temperature lower calcination 50min, natural cooling obtain water body chlorine residue adsorbent.
Comparative example 2
This comparative example prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;
S2. the diopside powder of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 700 DEG C of temperature lower calcinations 100min, natural cooling complete precalcining;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 1000 DEG C of temperature lower calcinations 50min, natural cooling;
S4. the diatomite powder of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 700 DEG C of temperature lower calcinations 100min, natural cooling complete precalcining;
S5. the precalcining product of step S4. is placed in porcelain crucible, is then placed in Muffle furnace in 1000 DEG C of temperature lower calcinations 50min, natural cooling;
S6. the product of step S3. and S5. are mixed, obtains water body chlorine residue adsorbent.
Wherein, the mass ratio of diopside powder and diatomite powder is 1: 4.
Comparative example 3
This comparative example the difference from embodiment 1 is that, diopside powder and diatomite powder can not cross 200 meshes, put down Equal partial size is about 100 μm;
Other experiment parameters and operation are same as Example 1.
Comparative example 4
This comparative example prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 4 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 600 DEG C of temperature lower calcinations 100min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 1000 DEG C of temperature lower calcinations 50min, natural cooling obtain water body chlorine residue adsorbent.
Comparative example 5
This comparative example prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 3 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 900 DEG C of temperature lower calcinations 100min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 900 DEG C of temperature lower calcinations 50min, natural cooling obtain water body chlorine residue adsorbent.
Comparative example 6
This comparative example prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 5 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 800 DEG C of temperature lower calcinations 120min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 800 DEG C of temperature lower calcinations 70min, natural cooling obtain water body chlorine residue adsorbent.
Comparative example 7
This comparative example prepares the method for water body chlorine residue adsorbent, and specific step is as follows:
S1. diopside and diatomite are ground in the ball mill respectively, crosses 200 meshes later, then dried at 90~110 DEG C It dries in case to constant weight, obtains diopside powder and diatomite powder;By diopside powder and diatomite powder in mass ratio 1: 4 Mixing, obtains mixture;
S2. the mixture of step S1. is placed in porcelain crucible, is then placed in Muffle furnace in 700 DEG C of temperature lower calcinations 100min, natural cooling obtain precalcining product;
S3. the precalcining product of step S2. is placed in porcelain crucible, is then placed in Muffle furnace in 1100 DEG C of temperature lower calcinations 50min, natural cooling obtain water body chlorine residue adsorbent.
Comparative example 8
Water body chlorine residue adsorbent is active carbon conventional in the art in this comparative example.
Performance test
(1) chlorine residue absorption property test method
Prepare the chlorine residue aqueous solution of chlorine residue initial concentration 5.0mg/L;
It is initially dense that chlorine residue is added in the conical flask of 250mL in the water body chlorine residue adsorbent for weighing 11.25g with electronic balance The 150mL chlorine residue aqueous solution of 5.0mg/L is spent, then the conical flask of solution is housed with black plastic bag package, conical flask is put into 30min is vibrated with 150rpm/min at 40 DEG C in water bath chader, 30min is centrifuged with the speed of 3000r/min after taking-up, from 0.45 μm of membrane filtration of supernatant after the heart, filtrate are used to analyze residual chlorine concentration.
Chlorine residue removal rate calculation method:
Chlorine residual measurement is using in " the drinking water standard method of inspection-disinfectant index " (GB/T5750.11-2006) It is easy to operate, using wider N, -1,4 phenylenediamine of N- diethyl (DPD) spectrophotometry.The chlorine residue mass concentration of measurement is trip From chlorine residue mass concentration.
Chlorine residue removal rate=(chlorine residue mass concentration after initial chlorine residue mass concentration-processing)/initial chlorine residue mass concentration.
Test result
The performance test results of the water body chlorine residue adsorbent of Examples 1 to 5 and comparative example 1~8 are as shown in table 1.
Water body chlorine residue adsorbent made from Examples 1 to 5 shows excellent chlorine residue adsorption capacity;Moreover, treated Water is in alkalescent, illustrates still to keep alkalescent after water body chlorine residue adsorbent adsorbs a certain amount of chlorine residue, is a kind of safe and healthy Water body chlorine residue adsorbent.Wherein, 1 chlorine residue absorption property of embodiment is best, is better than embodiment 4 and embodiment 5, it is seen that diopside Water body chlorine residue performance of the adsorbent obtained is preferable when the mass ratio of powder and diatomite powder is 1: 4, better than diopside powder and The mass ratio of diatomite powder is water body chlorine residue adsorbent prepared by 1: 3 or 1: 6.
And comparative example 1 is no by natural cooling after precalcining, water body chlorine residue performance of the adsorbent obtained is poor;It is right Ratio 2 calcines the method preparation remixed using two kinds of raw materials respectively, and chlorine residue absorption property is substantially reduced, it may be possible to two kinds of raw materials Certain compound action has occurred to the excellent water body chlorine residue adsorbent of forming properties.The grain diameter of comparative example 3 is larger, can not 200 meshes are crossed, the chlorine residue absorption property of water body chlorine residue adsorbent obtained is poor.The calcination temperature of comparative example 4~7 is too low or mistake Water body chlorine residue adsorbent of good performance can not be prepared in height.In comparative example 8, using conventional active carbon as water body Chlorine residue adsorbent has certain chlorine residue adsorption capacity, but treated that water is still weakly acidic, illustrates to a certain extent The problem of active carbon can gradually become slant acidity during adsorbing chlorine residue.
The performance of the water body chlorine residue adsorbent of 1 Examples 1 to 5 of table and comparative example 1~8
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention Protection scope within.

Claims (7)

1. a kind of preparation method of water body chlorine residue adsorbent, which comprises the steps of:
S1. it takes dry diopside powder and diatomite powder to be uniformly mixed, obtains mixture;The diopside powder and diatom Native powder crosses 200 meshes;
S2. by the mixture of step S1. in 700~800 DEG C of 100~120min of temperature lower calcination, then natural cooling, is obtained pre- Calcined product;
S3. the precalcining product of step S2. is obtained into the water body chlorine residue in 900~1000 DEG C of 50~70min of temperature lower calcination Adsorbent.
2. preparation method according to claim 1, which is characterized in that the quality of the diopside powder and diatomite powder Than being 1: (3~6).
3. preparation method according to claim 2, which is characterized in that the quality of the diopside powder and diatomite powder Than being 1: 4.
4. preparation method according to claim 1, which is characterized in that the diopside powder and diatomite powder of the drying It dries and obtains at a temperature of 90~110 DEG C after being ground respectively by diopside and diatomite.
5. the preparation method according to claim 4, which is characterized in that described grind is carried out by ball mill.
6. preparation method according to claim 1, which is characterized in that the calcining of step S1. and S2. are in Muffle furnace Middle progress, the mixture are placed in porcelain crucible.
7. water body chlorine residue adsorbent made from any one of claim 1~6 preparation method.
CN201910350906.9A 2019-04-28 2019-04-28 Water body residual chlorine adsorbent and preparation method thereof Active CN110124610B (en)

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