CN108176353A - There is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent and its preparation process of adsorption function to hardly degraded organic substance - Google Patents

There is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent and its preparation process of adsorption function to hardly degraded organic substance Download PDF

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CN108176353A
CN108176353A CN201810182562.0A CN201810182562A CN108176353A CN 108176353 A CN108176353 A CN 108176353A CN 201810182562 A CN201810182562 A CN 201810182562A CN 108176353 A CN108176353 A CN 108176353A
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mixed liquor
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temperature
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CN201810182562.0A
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高姌
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高姌
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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
    • B01J20/12Naturally occurring clays or bleaching 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
    • C02F2101/30Organic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/20Total organic carbon [TOC]

Abstract

The invention discloses a kind of PERFORMANCE OF MODIFIED VERMICULITE adsorbents to hardly degraded organic substance with adsorption function.The mixed liquor prepared after vermiculite cleaning through tetrabutylammonium chloride, 3 sulfopropyl hexadecyldimethyl benzyl ammonium ammoniums, calcium lignosulfonate and potassium oleate is modified to obtain substance L;The substance that the mixed liquor that substance L is prepared through tetramethylpiperidinol, diacetone alcohol, bicyclic oxygenated butadiene, diethy-aceto oxalate is modified is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent for having adsorption function to hardly degraded organic substance.The invention has the advantages that the PERFORMANCE OF MODIFIED VERMICULITE adsorbent prepared has many advantages, such as the hardly degraded organic substance in waste water adsorption efficiency is high, adsorption capacity is big.

Description

There is PERFORMANCE OF MODIFIED VERMICULITE adsorbent and its preparation of adsorption function to hardly degraded organic substance Technique

Technical field

It is more particularly to a kind of to there is adsorption function to change hardly degraded organic substance the invention belongs to wastewater treating technology field Property vermiculite absorbent 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 numerous and diverse, derives from many industries and neck Domain, such as petrochemical industry, organic chemical industry, printing and dyeing, rubber manufacture and pesticide.In 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 to utilize the metabolic processes of microorganism and endogenous respiration process, 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 chemisorbed, 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 and be efficiently used to adsorb Remove the sorbing material of hardly degraded organic substance.

Invention content

The object of the present invention is to provide a kind of PERFORMANCE OF MODIFIED VERMICULITE adsorbents to hardly degraded organic substance with adsorption function, prepare The technique of the adsorbent is as follows:

(1) after the 1000g vermiculites that grain size is 2~4cm are cleaned with tap water washes of absolute alcohol is used again, then use deionization Then water washing places 50 minutes in drying box of the temperature for 125 DEG C and obtains substance A;

(2) 0.052 gram of tetrabutylammonium chloride and 0.014 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In deionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor M1;

(3) substance A is added in mixed liquor M1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance B 1, and substance B 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance B;

(4) 1.58 grams of calcium lignosulfonates and 0.74 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor M2;

(5) substance B is added in mixed liquor M2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance C 1, and substance C 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance C;

(6) 0.048 gram of tetrabutylammonium chloride and 0.016 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In deionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N1;

(7) substance C is added in mixed liquor N1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance D1, and substance D1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance D;

(8) 1.55 grams of calcium lignosulfonates and 0.71 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor N2;

(9) substance D is added in mixed liquor N2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance E1, and substance E1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance E;

(10) 0.044 gram of tetrabutylammonium chloride and 0.018 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to In 3000mL deionized waters, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O1;

(11) substance E is added in mixed liquor O1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance F1, and substance F1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance F;

(12) 1.52 grams of calcium lignosulfonates and 0.68 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor O2;

(13) substance F is added in mixed liquor O2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance G1, and substance G1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance G;

(14) 0.040 gram of tetrabutylammonium chloride and 0.020 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to In 3000mL deionized waters, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor P1;

(15) substance G is added in mixed liquor P1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance H1, and substance H1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance H;

(16) 1.49 grams of calcium lignosulfonates and 0.65 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor P2;

(17) substance H is added in mixed liquor P2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance J1, and substance J1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance J;

(18) 0.036 gram of tetrabutylammonium chloride and 0.022 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to In 3000mL deionized waters, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1;

(19) substance J is added in mixed liquor Q1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance K1, and substance K1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance K;

(20) 1.46 grams of calcium lignosulfonates and 0.62 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor Q2;

(21) substance K is added in mixed liquor Q2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance L1, and substance L1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance L;

(22) 5.7 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor R1;

(23) 7.6 grams of diacetone alcohol and 4.7 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S1;

(24) mixed liquor S1 and 2.3 grams of diethy-aceto oxalates are added in mixed liquor R1, are stirred under the conditions of 1000r/min 3 minutes, obtain mixed liquor T1;

(25) substance L is added in mixed liquor T1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance M1, and substance M1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance M;

(26) 5.2 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor R2;

(27) 7.1 grams of diacetone alcohol and 4.2 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S2;

(28) mixed liquor S2 and 2.0 grams of diethy-aceto oxalates are added in mixed liquor R2, are stirred under the conditions of 1000r/min 3 minutes, obtain mixed liquor T2;

(29) substance M is added in mixed liquor T2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance N1, and substance N1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance O;

(30) 4.7 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor R3;

(31) 6.6 grams of diacetone alcohol and 3.7 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S3;

(32) mixed liquor S3 and 1.7 grams of diethy-aceto oxalates are added in mixed liquor R3, are stirred under the conditions of 1000r/min 3 minutes, obtain mixed liquor T3;

(33) substance O is added in mixed liquor T3, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains Substance P 1, and Substance P 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains Substance P;

(34) 4.2 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor R4;

(35) 6.1 grams of diacetone alcohol and 3.2 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S4;

(36) mixed liquor S4 and 1.4 grams of diethy-aceto oxalates are added in mixed liquor R4, are stirred under the conditions of 1000r/min 3 minutes, obtain mixed liquor T4;

(37) Substance P is added in mixed liquor T4, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance Q1, substance Q1 is placed 35 minutes in drying box of the temperature for 80 DEG C, obtained substance is to difficult to degrade Organic matter has the PERFORMANCE OF MODIFIED VERMICULITE adsorbent of adsorption function.

The invention has the advantages that the PERFORMANCE OF MODIFIED VERMICULITE adsorbent prepared has absorption to the hardly degraded organic substance in waste water Efficient, the advantages that adsorption capacity is big.

Specific embodiment

Embodiment

The PERFORMANCE OF MODIFIED VERMICULITE adsorbent for having adsorption function to hardly degraded organic substance is prepared by following process:

1) after the 1000g vermiculites that grain size is 2~4cm are cleaned with tap water washes of absolute alcohol is used again, then use deionization Then water washing places 50 minutes in drying box of the temperature for 125 DEG C and obtains substance A;

2) 0.052 gram of tetrabutylammonium chloride and 0.014 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In deionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor M1;

3) substance A is added in mixed liquor M1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Substance B 1 is obtained, substance B 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance B;

4) 1.58 grams of calcium lignosulfonates and 0.74 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor M2;

5) substance B is added in mixed liquor M2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Substance C 1 is obtained, substance C 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance C;

6) 0.048 gram of tetrabutylammonium chloride and 0.016 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In deionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N1;

7) substance C is added in mixed liquor N1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Substance D1 is obtained, substance D1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance D;

8) 1.55 grams of calcium lignosulfonates and 0.71 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor N2;

9) substance D is added in mixed liquor N2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Substance E1 is obtained, substance E1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance E;

10) 0.044 gram of tetrabutylammonium chloride and 0.018 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In deionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O1;

11) substance E is added in mixed liquor O1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance F1, and substance F1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance F;

12) 1.52 grams of calcium lignosulfonates and 0.68 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor O2;

13) substance F is added in mixed liquor O2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance G1, and substance G1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance G;

14) 0.040 gram of tetrabutylammonium chloride and 0.020 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In deionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor P1;

15) substance G is added in mixed liquor P1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance H1, and substance H1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance H;

16) 1.49 grams of calcium lignosulfonates and 0.65 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor P2;

17) substance H is added in mixed liquor P2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance J1, and substance J1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance J;

18) 0.036 gram of tetrabutylammonium chloride and 0.022 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In deionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1;

19) substance J is added in mixed liquor Q1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance K1, and substance K1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance K;

20) 1.46 grams of calcium lignosulfonates and 0.62 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor Q2;

21) substance K is added in mixed liquor Q2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance L1, and substance L1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance L;

22) 5.7 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor R1;

23) 7.6 grams of diacetone alcohol and 4.7 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S1;

24) mixed liquor S1 and 2.3 grams of diethy-aceto oxalates are added in mixed liquor R1,3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor T1;

25) substance L is added in mixed liquor T1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance M1, and substance M1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance M;

26) 5.2 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor R2;

27) 7.1 grams of diacetone alcohol and 4.2 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S2;

28) mixed liquor S2 and 2.0 grams of diethy-aceto oxalates are added in mixed liquor R2,3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor T2;

29) substance M is added in mixed liquor T2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance N1, and substance N1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance O;

30) 4.7 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor R3;

31) 6.6 grams of diacetone alcohol and 3.7 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S3;

32) mixed liquor S3 and 1.7 grams of diethy-aceto oxalates are added in mixed liquor R3,3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor T3;

33) substance O is added in mixed liquor T3, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains Substance P 1, and Substance P 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains Substance P;

34) 4.2 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor R4;

35) 6.1 grams of diacetone alcohol and 3.2 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/ It is stirred 3 minutes under the conditions of min, obtains mixed liquor S4;

36) mixed liquor S4 and 1.4 grams of diethy-aceto oxalates are added in mixed liquor R4,3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor T4;

37) Substance P is added in mixed liquor T4, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid Body obtains substance Q1, substance Q1 is placed 35 minutes in drying box of the temperature for 80 DEG C, obtained substance is to difficult to degrade Organic matter has the PERFORMANCE OF MODIFIED VERMICULITE adsorbent of adsorption function.

There is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent of adsorption function to containing to hardly degraded organic substance with made from the method for the present invention The waste water of hardly degraded organic substance has carried out adsorption Removal, the results showed that:Into the waste water that 1000 milliliters of TOC are 245mg/L 3.8 grams of PERFORMANCE OF MODIFIED VERMICULITE adsorbents are added, the TOC during absorption is discharged after 6 minutes is reduced to 2.1mg/L.

Claims (1)

1. a kind of PERFORMANCE OF MODIFIED VERMICULITE adsorbent to hardly degraded organic substance with adsorption function, which is characterized in that prepare the adsorbent Technique it is as follows:
(1) after the 1000g vermiculites that grain size is 2~4cm are cleaned with tap water washes of absolute alcohol is used again, then be washed with deionized water It washs, is placed 50 minutes in the drying box for being then 125 DEG C in temperature and obtain substance A;
(2) by 0.052 gram of tetrabutylammonium chloride and 0.014 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium be added to 3000mL go from In sub- water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor M1;
(3) substance A is added in mixed liquor M1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance B 1, substance B 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance B;
(4) 1.58 grams of calcium lignosulfonates and 0.74 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/min items It is stirred 3 minutes under part, obtains mixed liquor M2;
(5) substance B is added in mixed liquor M2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance C 1, substance C 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance C;
(6) by 0.048 gram of tetrabutylammonium chloride and 0.016 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium be added to 3000mL go from In sub- water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N1;
(7) substance C is added in mixed liquor N1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance D1, substance D1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance D;
(8) 1.55 grams of calcium lignosulfonates and 0.71 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/min items It is stirred 3 minutes under part, obtains mixed liquor N2;
(9) substance D is added in mixed liquor N2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance E1, substance E1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance E;
(10) 0.044 gram of tetrabutylammonium chloride and 0.018 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In ionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O1;
(11) substance E is added in mixed liquor O1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance F1, substance F1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance F;
(12) 1.52 grams of calcium lignosulfonates and 0.68 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor O2;
(13) substance F is added in mixed liquor O2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance G1, substance G1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance G;
(14) 0.040 gram of tetrabutylammonium chloride and 0.020 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In ionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor P1;
(15) substance G is added in mixed liquor P1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance H1, substance H1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance H;
(16) 1.49 grams of calcium lignosulfonates and 0.65 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor P2;
(17) substance H is added in mixed liquor P2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance J1, substance J1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance J;
(18) 0.036 gram of tetrabutylammonium chloride and 0.022 gram of 3- sulfopropyl hexadecyldimethyl benzyl ammonium ammonium are added to 3000mL In ionized water, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1;
(19) substance J is added in mixed liquor Q1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance K1, substance K1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance K;
(20) 1.46 grams of calcium lignosulfonates and 0.62 gram of potassium oleate are added in 3000mL deionized waters, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q2;
(21) substance K is added in mixed liquor Q2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance L1, substance L1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance L;
(22) 5.7 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, are stirred 3 minutes under the conditions of 1000r/min, Obtain mixed liquor R1;
(23) 7.6 grams of diacetone alcohol and 4.7 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/min items It is stirred 3 minutes under part, obtains mixed liquor S1;
(24) mixed liquor S1 and 2.3 grams of diethy-aceto oxalates are added in mixed liquor R1,3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor T1;
(25) substance L is added in mixed liquor T1, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance M1, substance M1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance M;
(26) 5.2 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, are stirred 3 minutes under the conditions of 1000r/min, Obtain mixed liquor R2;
(27) 7.1 grams of diacetone alcohol and 4.2 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/min items It is stirred 3 minutes under part, obtains mixed liquor S2;
(28) mixed liquor S2 and 2.0 grams of diethy-aceto oxalates are added in mixed liquor R2,3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor T2;
(29) substance M is added in mixed liquor T2, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance N1, substance N1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains substance O;
(30) 4.7 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, are stirred 3 minutes under the conditions of 1000r/min, Obtain mixed liquor R3;
(31) 6.6 grams of diacetone alcohol and 3.7 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/min items It is stirred 3 minutes under part, obtains mixed liquor S3;
(32) mixed liquor S3 and 1.7 grams of diethy-aceto oxalates are added in mixed liquor R3,3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor T3;
(33) substance O is added in mixed liquor T3, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To Substance P 1, Substance P 1 in drying box of the temperature for 80 DEG C is placed 35 minutes, obtains Substance P;
(34) 4.2 grams of tetramethylpiperidinols are added in 2000mL absolute ethyl alcohols, are stirred 3 minutes under the conditions of 1000r/min, Obtain mixed liquor R4;
(35) 6.1 grams of diacetone alcohol and 3.2 grams of bicyclic oxygenated butadienes are added in 150mL isopropanols, in 1000r/min items It is stirred 3 minutes under part, obtains mixed liquor S4;
(36) mixed liquor S4 and 1.4 grams of diethy-aceto oxalates are added in mixed liquor R4,3 points is stirred under the conditions of 1000r/min Clock obtains mixed liquor T4;
(37) Substance P is added in mixed liquor T4, is shaken 45 minutes in the shaking table for being 33 DEG C in temperature, be filtered to remove liquid and obtain To substance Q1, substance Q1 is placed 35 minutes in drying box of the temperature for 80 DEG C, obtained substance is to difficult to degrade organic Object has the PERFORMANCE OF MODIFIED VERMICULITE adsorbent of adsorption function.
CN201810182562.0A 2018-03-06 2018-03-06 There is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent and its preparation process of adsorption function to hardly degraded organic substance CN108176353A (en)

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