CN108339519A - Modified activated carbon absorbent and its preparation process for Adsorption hardly degraded organic substance - Google Patents
Modified activated carbon absorbent and its preparation process for Adsorption hardly degraded organic substance Download PDFInfo
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- CN108339519A CN108339519A CN201810182823.9A CN201810182823A CN108339519A CN 108339519 A CN108339519 A CN 108339519A CN 201810182823 A CN201810182823 A CN 201810182823A CN 108339519 A CN108339519 A CN 108339519A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
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Abstract
The invention discloses a kind of modified activated carbon absorbents for Adsorption hardly degraded organic substance.Through NbCl after activated carbon cleaning4、ZnCl2、Cu(NO3)2With Mg (NO3)2The mixed liquor of preparation is modified to obtain substance B；The mixed liquor that substance B is prepared through sodium aluminate, ammonium hexafluorophosphate, potassium borohydride and lithium chloride is modified to obtain substance D；The modified obtained substance of mixed liquor that substance D is prepared through tert-butyl chloro-silicane, cyclohexyl formaldehyde, phenyltrimethoxysila,e, p-methyl benzenesulfonic acid tetrafluoro propyl ester and hydroxypropyl B cyclodextrin is the modified activated carbon absorbent for Adsorption hardly degraded organic substance.The invention has the advantages that the modified activated carbon absorbent prepared has many advantages, such as that adsorption efficiency is high, adsorption capacity is big to the hardly degraded organic substance in waste water.
Description
Technical field
The invention belongs to wastewater treating technology fields, more particularly to a kind of modification for Adsorption hardly degraded organic substance
Acticarbon and its preparation process.
Background technology
In recent years, with the fast development of modern industrial or agricultural, wastewater discharge is caused increasingly to increase, and contained dirt in waste water
The ingredient of dye object is constantly complicated with type, wherein containing such as phenolic compound, organochlorine compound, organophosphorus pesticide, more chlorine
The organic pollutions such as biphenyl, polycyclic aromatic hydrocarbon, nitro compound, organic dyestuff, incretion interferent, surfactant, it is serious to endanger
Do harm to the living environment of the mankind.Hardly degraded organic substance general toxicity is all larger, some pollutants have " three cause " effect (teratogenesis,
Carcinogenic, mutagenesis), stability is strong, and microbial degradation speed is slow or even non-degradable, so that conventional water treatment technology is (main
To be biological oxidation process) it is difficult to remove it, these harmful organic substances are detained in water body and soil and are difficult to disappear for a long time, right
Human body brings severe potential hazard.Hardly degraded organic substance belongs to artificial-synthetic compound mostly, and since the mankind are to artificial
The demand face for synthesizing compound is wider, therefore causes the type of hardly degraded organic substance more and complicated, derives from many industries and neck
Domain, such as petrochemical industry, organic chemical industry, printing and dyeing, rubber manufacture and pesticide.Many places in China, due to a lack of effectively controlling
Reason technology and environmental protection theory, many organic wastewater with difficult degradation thereby cause serious ring without being effectively treated and direct emission
Border is polluted and the dirty hidden danger of long-term cause, and great threat is formed to health and the ecosystem.Therefore, organic wastewater with difficult degradation thereby is handled
As the difficult point and hot spot in current environmental pollution improvement and control problem.
It is more to the processing method of persistent organic pollutants in water, after its compressive classification, mainly there are chemical method, biology
Method and physico-chemical process.Chemical oxidation techniques are the oxidation and catalytic action using oxidant, it is made to be sent out with hardly degraded organic substance
Raw reaction so that its preliminary exposition and stabilization, reduce its bio-toxicity, and improves hardly degraded organic substance follow-up to a certain extent
Biodegradability in biological treatment.Bioanalysis is the metabolic processes and endogenous respiration process using microorganism, absorption, product
Organic pollution poly-, in oxygenolysis water, but when containing persistent organic pollutants in waste water, microorganism degrade to it speed
Degree can not even degrade slowly, it is difficult to which the concentration of hardly degraded organic substance to be reached to the level of environmental requirement.Therefore, environmental-friendly,
Low-carbon saving and the hotspot approach that treatment process is simple, high treating effect physico-chemical process is increasingly becoming processing hardly degraded organic substance,
The technique of physico-chemical process processing organic wastewater with difficult degradation thereby mainly has absorption, membrane filter method etc..Wherein, absorption method mainly passes through
The removal to organic wastewater with difficult degradation thereby, adsorption process are realized with the adsorbent for having abundant pore structure or large specific surface area
Including adsorpting types such as chemisorption, physical absorption, exchange adsorptions, adsorption effect sorbent suspension surface chemical property and structure are special
The influence and restriction of the factors such as point, adsorption molecule size and its physico-chemical property, absorption environment.
Absorption method has many advantages, such as that adsorption efficiency is high, process equipment is simple, floor space is small, consumptive material is cheap and easily-available, but big
Most adsorbents have Selective adsorption, can improve its absorption property, Jin Ergai by the way that adsorbent is the means such as to be modified to
The kind removal ability to hardly degraded organic substance.But generally adsorbent is expensive, regeneration rate is not high.Therefore, seek a kind of high
Adsorbent imitate, that adsorption capacity is big, regeneration rate is high is the emphasis for adsorbing research field.Also lack at present efficient for adsorbing
Remove the sorbing material of hardly degraded organic substance.
Invention content
The object of the present invention is to provide a kind of modified activated carbon absorbents for Adsorption hardly degraded organic substance, prepare
The technique of the adsorbent is as follows：
(1) by grain size be 1~2cm 1000g activated carbons cleaned with tap water after again use washes of absolute alcohol, then spend from
Then sub- water washing places 50 minutes in the drying box that temperature is 125 DEG C and obtains substance A；
(2) by 8.65 grams of NbCl4With 2.68 grams of ZnCl2It is added in 8000mL deionized waters, under the conditions of 1000r/min
Stirring 3 minutes, is divided into 4 parts of equivalent, obtains mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor H4 after shaking up；
(3) it is the Cu (NO of 0.88mol/L by 140mL molar concentrations3)2Solution and 60mL molar concentrations are 0.52mol/L's
Mg(NO3)2Solution is added in mixed liquor H1, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Body obtains substance B 1, and substance B 1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 2；
(5) it is the Cu (NO of 0.88mol/L by 120mL molar concentrations3)2Solution and 80mL molar concentrations are 0.52mol/L's
Mg(NO3)2Solution is added in mixed liquor H2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Body obtains substance B 3, and substance B 3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 4；
(7) it is the Cu (NO of 0.88mol/L by 100mL molar concentrations3)2Solution and 100mL molar concentrations are 0.52mol/L
Mg (NO3)2Solution is added in mixed liquor H3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Body obtains substance B 5, and substance B 5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 6；
(9) it is the Cu (NO of 0.88mol/L by 80mL molar concentrations3)2Solution and 120mL molar concentrations are 0.52mol/L's
Mg(NO3)2Solution is added in mixed liquor H4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, shakes 40 minutes, is filtered to remove in the shaking table that temperature is 35 DEG C
Liquid obtains substance B 7, and substance B 7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B；
(11) 5.6 grams of sodium aluminates and 8.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor J1；
(12) substance B is added in mixed liquor J1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance C 1, and substance C 1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 2；
(13) 1.22 grams of potassium borohydrides and 0.56 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor K1；
(14) substance C 2 is added in mixed liquor K1, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance D1, and substance D1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D2；
(15) 5.1 grams of sodium aluminates and 8.3 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor J2；
(16) substance D2 is added in mixed liquor J2, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance C 3, and substance C 3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 4；
(17) 1.18 grams of potassium borohydrides and 0.52 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor K2；
(18) substance C 4 is added in mixed liquor K2, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance D3, and substance D3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D4；
(19) 4.6 grams of sodium aluminates and 7.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor J3；
(20) substance D4 is added in mixed liquor J3, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance C 5, and substance C 5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 6；
(21) 1.14 grams of potassium borohydrides and 0.48 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor K3；
(22) substance C 6 is added in mixed liquor K3, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance D5, and substance D5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D6；
(23) 4.1 grams of sodium aluminates and 7.3 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor J4；
(24) substance D6 is added in mixed liquor J4, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance C 7, and substance C 7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 8；
(25) 1.10 grams of potassium borohydrides and 0.44 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor K4；
(26) substance C 8 is added in mixed liquor K4, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance D7, and substance D7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D8；
(27) 3.6 grams of sodium aluminates and 6.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor J5；
(28) substance D8 is added in mixed liquor J5, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance C 9, and substance C 9 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 10；
(29) 1.06 grams of potassium borohydrides and 0.40 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor K5；
(30) substance C 10 is added in mixed liquor K5, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance D9, and substance D9 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D；
(31) 7.3 grams of tert-butyl chloro-silicanes and 8.6 grams of cyclohexyl formaldehyde are added to 9000mL absolute ethyl alcohols
In, it is stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor L1, mixed liquor L2, mixed liquor
L3, mixed liquor L4；
(32) 9.9 grams of phenyltrimethoxysila,es and 7.1 grams of p-methyl benzenesulfonic acid tetrafluoro propyl ester are added to 800mL chloroforms
In, it is stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor
M3, mixed liquor M4；
(33) mixed liquor M1 and 2.4 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor N1；
(34) substance D is added in mixed liquor N1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance E1, and substance E1 is placed 45 minutes in 85 DEG C of drying box, obtains substance E2；
(35) mixed liquor M2 and 2.2 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor N2；
(36) substance E2 is added in mixed liquor N2, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance E3, and substance E3 is placed 45 minutes in 85 DEG C of drying box, obtains substance E4；
(37) mixed liquor M3 and 2.0 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor N3；
(38) substance E4 is added in mixed liquor N3, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance E5, and substance E5 is placed 45 minutes in 85 DEG C of drying box, obtains substance E6；
(39) mixed liquor M4 and 1.8 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L4, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor N4；
(40) substance E6 is added in mixed liquor N4, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance E7, and substance E7 is placed 45 minutes in 85 DEG C of drying box, and obtained substance is to be used for Adsorption
The modified activated carbon absorbent of hardly degraded organic substance.
It is inhaled the invention has the advantages that the modified activated carbon absorbent prepared has the hardly degraded organic substance in waste water
The advantages that attached efficient, adsorption capacity is big.
Specific implementation mode
Embodiment
Modified activated carbon absorbent for Adsorption hardly degraded organic substance is prepared by following process：
1) by grain size be 1~2cm 1000g activated carbons cleaned with tap water after again use washes of absolute alcohol, then spend from
Then sub- water washing places 50 minutes in the drying box that temperature is 125 DEG C and obtains substance A；
2) by 8.65 grams of NbCl4With 2.68 grams of ZnCl2It is added in 8000mL deionized waters, is stirred under the conditions of 1000r/min
It mixes 3 minutes, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor H4；
3) it is the Cu (NO of 0.88mol/L by 140mL molar concentrations3)2Solution and 60mL molar concentrations are 0.52mol/L's
Mg(NO3)2Solution is added in mixed liquor H1, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J1；
4) substance A is added in mixed liquor J1, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Substance B 1 is obtained, substance B 1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 2；
5) it is the Cu (NO of 0.88mol/L by 120mL molar concentrations3)2Solution and 80mL molar concentrations are 0.52mol/L's
Mg(NO3)2Solution is added in mixed liquor H2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J2；
6) substance B 2 is added in mixed liquor J2, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Body obtains substance B 3, and substance B 3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 4；
7) it is the Cu (NO of 0.88mol/L by 100mL molar concentrations3)2Solution and 100mL molar concentrations are 0.52mol/L's
Mg(NO3)2Solution is added in mixed liquor H3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J3；
8) substance B 4 is added in mixed liquor J3, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Body obtains substance B 5, and substance B 5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 6；
9) it is the Cu (NO of 0.88mol/L by 80mL molar concentrations3)2Solution and 120mL molar concentrations are 0.52mol/L's
Mg(NO3)2Solution is added in mixed liquor H4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J4；
10) substance B 6 is added in mixed liquor J4, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Body obtains substance B 7, and substance B 7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B；
11) 5.6 grams of sodium aluminates and 8.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor J1；
12) substance B is added in mixed liquor J1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance C 1, and substance C 1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 2；
13) 1.22 grams of potassium borohydrides and 0.56 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K1；
14) substance C 2 is added in mixed liquor K1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance D1, and substance D1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D2；
15) 5.1 grams of sodium aluminates and 8.3 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor J2；
16) substance D2 is added in mixed liquor J2, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance C 3, and substance C 3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 4；
17) 1.18 grams of potassium borohydrides and 0.52 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K2；
18) substance C 4 is added in mixed liquor K2, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance D3, and substance D3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D4；
19) 4.6 grams of sodium aluminates and 7.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor J3；
20) substance D4 is added in mixed liquor J3, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance C 5, and substance C 5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 6；
21) 1.14 grams of potassium borohydrides and 0.48 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K3；
22) substance C 6 is added in mixed liquor K3, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance D5, and substance D5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D6；
23) 4.1 grams of sodium aluminates and 7.3 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor J4；
24) substance D6 is added in mixed liquor J4, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance C 7, and substance C 7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 8；
25) 1.10 grams of potassium borohydrides and 0.44 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K4；
26) substance C 8 is added in mixed liquor K4, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance D7, and substance D7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D8；
27) 3.6 grams of sodium aluminates and 6.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor J5；
28) substance D8 is added in mixed liquor J5, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance C 9, and substance C 9 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 10；
29) 1.06 grams of potassium borohydrides and 0.40 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor K5；
30) substance C 10 is added in mixed liquor K5, shakes 45 minutes, is filtered to remove in the shaking table that temperature is 33 DEG C
Liquid obtains substance D9, and substance D9 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D；
31) 7.3 grams of tert-butyl chloro-silicanes and 8.6 grams of cyclohexyl formaldehyde are added to 9000mL absolute ethyl alcohols
In, it is stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor L1, mixed liquor L2, mixed liquor
L3, mixed liquor L4；
32) 9.9 grams of phenyltrimethoxysila,es and 7.1 grams of p-methyl benzenesulfonic acid tetrafluoro propyl ester are added in 800mL chloroforms,
Stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent be divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3,
Mixed liquor M4；
33) mixed liquor M1 and 2.4 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L1, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor N1；
34) substance D is added in mixed liquor N1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance E1, and substance E1 is placed 45 minutes in 85 DEG C of drying box, obtains substance E2；
35) mixed liquor M2 and 2.2 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L2, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor N2；
36) substance E2 is added in mixed liquor N2, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance E3, and substance E3 is placed 45 minutes in 85 DEG C of drying box, obtains substance E4；
37) mixed liquor M3 and 2.0 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L3, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor N3；
38) substance E4 is added in mixed liquor N3, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance E5, and substance E5 is placed 45 minutes in 85 DEG C of drying box, obtains substance E6；
39) mixed liquor M4 and 1.8 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L4, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor N4；
40) substance E6 is added in mixed liquor N4, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Body obtains substance E7, and substance E7 is placed 45 minutes in 85 DEG C of drying box, and obtained substance is difficult for Adsorption
The modified activated carbon absorbent of degradation of organic substances.
With made from the method for the present invention be used for Adsorption hardly degraded organic substance modified activated carbon absorbent to containing
The waste water of hardly degraded organic substance has carried out adsorption Removal, the results showed that：In the waste water for being 245mg/L to 1000 milliliters of TOC
3.8 grams of modified activated carbon absorbents are added, the TOC during absorption is discharged after 6 minutes is reduced to 3.8mg/L.
Claims (1)
1. a kind of modified activated carbon absorbent for Adsorption hardly degraded organic substance, which is characterized in that prepare the adsorbent
Technique it is as follows：
(1) washes of absolute alcohol is used again after cleaning the 1000g activated carbons that grain size is 1~2cm with tap water, then uses deionized water
Then washing places 50 minutes in the drying box that temperature is 125 DEG C and obtains substance A；
(2) by 8.65 grams of NbCl4With 2.68 grams of ZnCl2It is added in 8000mL deionized waters, 3 is stirred under the conditions of 1000r/min
Minute, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor H4；
(3) it is the Cu (NO of 0.88mol/L by 140mL molar concentrations3)2Solution and the Mg that 60mL molar concentrations are 0.52mol/L
(NO3)2Solution is added in mixed liquor H1, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid and obtains
To substance B 1, substance B 1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 2；
(5) it is the Cu (NO of 0.88mol/L by 120mL molar concentrations3)2Solution and the Mg that 80mL molar concentrations are 0.52mol/L
(NO3)2Solution is added in mixed liquor H2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid and obtains
To substance B 3, substance B 3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 4；
(7) it is the Cu (NO of 0.88mol/L by 100mL molar concentrations3)2Solution and the Mg that 100mL molar concentrations are 0.52mol/L
(NO3)2Solution is added in mixed liquor H3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid and obtains
To substance B 5, substance B 5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B 6；
(9) it is the Cu (NO of 0.88mol/L by 80mL molar concentrations3)2Solution and the Mg that 120mL molar concentrations are 0.52mol/L
(NO3)2Solution is added in mixed liquor H4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, is shaken 40 minutes in the shaking table that temperature is 35 DEG C, is filtered to remove liquid
Substance B 7 is obtained, substance B 7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance B；
(11) 5.6 grams of sodium aluminates and 8.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor J1；
(12) substance B is added in mixed liquor J1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid and obtains
To substance C 1, substance C 1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 2；
(13) 1.22 grams of potassium borohydrides and 0.56 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K1；
(14) substance C 2 is added in mixed liquor K1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance D1 is obtained, substance D1 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D2；
(15) 5.1 grams of sodium aluminates and 8.3 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor J2；
(16) substance D2 is added in mixed liquor J2, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance C 3 is obtained, substance C 3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 4；
(17) 1.18 grams of potassium borohydrides and 0.52 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K2；
(18) substance C 4 is added in mixed liquor K2, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance D3 is obtained, substance D3 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D4；
(19) 4.6 grams of sodium aluminates and 7.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor J3；
(20) substance D4 is added in mixed liquor J3, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance C 5 is obtained, substance C 5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 6；
(21) 1.14 grams of potassium borohydrides and 0.48 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K3；
(22) substance C 6 is added in mixed liquor K3, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance D5 is obtained, substance D5 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D6；
(23) 4.1 grams of sodium aluminates and 7.3 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor J4；
(24) substance D6 is added in mixed liquor J4, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance C 7 is obtained, substance C 7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 8；
(25) 1.10 grams of potassium borohydrides and 0.44 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K4；
(26) substance C 8 is added in mixed liquor K4, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance D7 is obtained, substance D7 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D8；
(27) 3.6 grams of sodium aluminates and 6.8 grams of ammonium hexafluorophosphates are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor J5；
(28) substance D8 is added in mixed liquor J5, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance C 9 is obtained, substance C 9 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance C 10；
(29) 1.06 grams of potassium borohydrides and 0.40 grams lithium chloride are added in 3000mL deionized waters, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor K5；
(30) substance C 10 is added in mixed liquor K5, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance D9 is obtained, substance D9 is placed 40 minutes in the drying box that temperature is 195 DEG C, obtains substance D；
(31) 7.3 grams of tert-butyl chloro-silicanes and 8.6 grams of cyclohexyl formaldehyde are added in 9000mL absolute ethyl alcohols,
It is stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtained mixed liquor L1, mixed liquor L2, mixed liquor L3, mix
Close liquid L4；
(32) 9.9 grams of phenyltrimethoxysila,es and 7.1 grams of p-methyl benzenesulfonic acid tetrafluoro propyl ester are added in 800mL chloroforms,
It is stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtained mixed liquor M1, mixed liquor M2, mixed liquor M3, mix
Close liquid M4；
(33) mixed liquor M1 and 2.4 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L1, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N1；
(34) substance D is added in mixed liquor N1, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid and obtains
To substance E1, substance E1 is placed 45 minutes in 85 DEG C of drying box, obtains substance E2；
(35) mixed liquor M2 and 2.2 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L2, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N2；
(36) substance E2 is added in mixed liquor N2, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance E3 is obtained, substance E3 is placed 45 minutes in 85 DEG C of drying box, obtains substance E4；
(37) mixed liquor M3 and 2.0 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L3, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N3；
(38) substance E4 is added in mixed liquor N3, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance E5 is obtained, substance E5 is placed 45 minutes in 85 DEG C of drying box, obtains substance E6；
(39) mixed liquor M4 and 1.8 grams of hydroxypropyl-B- cyclodextrin are added in mixed liquor L4, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor N4；
(40) substance E6 is added in mixed liquor N4, is shaken 45 minutes in the shaking table that temperature is 33 DEG C, is filtered to remove liquid
Substance E7 is obtained, substance E7 is placed 45 minutes in 85 DEG C of drying box, obtained substance is to be dropped for Adsorption difficulty
Solve the modified activated carbon absorbent of organic matter.
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| CN113198432A (en) * | 2021-06-18 | 2021-08-03 | 江苏乾汇和环保再生有限公司 | Preparation method of biomass activated carbon |
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