CN107668034A - A kind of biological material for solidifying quaternary ammonium salt and preparation method and application - Google Patents
A kind of biological material for solidifying quaternary ammonium salt and preparation method and application Download PDFInfo
- Publication number
- CN107668034A CN107668034A CN201710945437.6A CN201710945437A CN107668034A CN 107668034 A CN107668034 A CN 107668034A CN 201710945437 A CN201710945437 A CN 201710945437A CN 107668034 A CN107668034 A CN 107668034A
- Authority
- CN
- China
- Prior art keywords
- biological material
- quaternary ammonium
- ammonium salt
- stirring reaction
- content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 150000003242 quaternary ammonium salts Chemical class 0.000 title claims abstract description 56
- 239000012620 biological material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 7
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 34
- -1 alkyl dimethyl tertiary amides Chemical class 0.000 claims description 26
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 241000209140 Triticum Species 0.000 claims description 15
- 235000021307 Triticum Nutrition 0.000 claims description 15
- 238000004659 sterilization and disinfection Methods 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 239000010902 straw Substances 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 240000008042 Zea mays Species 0.000 claims description 8
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000002585 base Substances 0.000 claims description 7
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 6
- 235000009973 maize Nutrition 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical class CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 5
- 240000007594 Oryza sativa Species 0.000 claims description 5
- 235000007164 Oryza sativa Nutrition 0.000 claims description 5
- 230000001172 regenerating effect Effects 0.000 claims description 5
- 235000009566 rice Nutrition 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 150000003512 tertiary amines Chemical class 0.000 claims description 5
- 150000001447 alkali salts Chemical class 0.000 claims description 4
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 3
- 235000018262 Arachis monticola Nutrition 0.000 claims description 3
- 241001494508 Arundo donax Species 0.000 claims description 3
- 235000014676 Phragmites communis Nutrition 0.000 claims description 3
- 244000269722 Thea sinensis Species 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 235000020232 peanut Nutrition 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 244000068988 Glycine max Species 0.000 claims description 2
- 235000010469 Glycine max Nutrition 0.000 claims description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 2
- 235000005822 corn Nutrition 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 229910001415 sodium ion Inorganic materials 0.000 claims description 2
- 239000010977 jade Substances 0.000 claims 1
- 241000894006 Bacteria Species 0.000 abstract description 17
- 238000013459 approach Methods 0.000 abstract description 3
- 244000052769 pathogen Species 0.000 abstract description 3
- 230000001717 pathogenic effect Effects 0.000 abstract description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 38
- 239000003899 bactericide agent Substances 0.000 description 35
- 239000002028 Biomass Substances 0.000 description 31
- 239000000463 material Substances 0.000 description 17
- 230000000694 effects Effects 0.000 description 15
- 239000002384 drinking water standard Substances 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- 230000001954 sterilising effect Effects 0.000 description 10
- 241000588724 Escherichia coli Species 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 4
- 239000002154 agricultural waste Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical class CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- QDYLMAYUEZBUFO-UHFFFAOYSA-N cetalkonium chloride Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 QDYLMAYUEZBUFO-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical class CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 1
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000002068 microbial inoculum Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000006385 ozonation reaction Methods 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/12—Quaternary ammonium compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- 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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of biological material for solidifying quaternary ammonium salt and preparation method and application, the biological material surface cure has quaternary ammonium group；The chemical formula of quaternary ammonium group is：−N+R(CH3)2, wherein, R C8H17、−C10H21、−C12H25、−C14H29Or C16H33；The content of quaternary ammonium group is 0.1 ~ 1.4 mmol/g.The biological material that the present invention is prepared, is expected to succinct, the efficient deep purifying realized to bacterium in water and pathogen, and the improvement of advanced treating and Polluted raw water for biochemical tail water provides new approaches, there is preferable novelty.
Description
Technical field
Biomass-based immobilization quaternary ammonium salt is prepared the present invention relates to one kind as primary raw material by the use of agricultural waste material to kill
The method of microbial inoculum, belong to changing waste into resources utilization and water body disinfection process field.
Background technology
In general, although the microorganism of the water outlet 90% ~ 99% after biochemical treatment is effectively removed, bacterium it is absolute
Quantity is still very considerable, and amount of total colibacillus is average 104~105Between individual/L, and pathogen be present, they may be by direct
The approach such as contact, aerosol are propagated and produce public health security risk.Therefore, effective sterilization of biochemical tail water is to receiving water body
Environmental security it is most important.
Biochemical tail water sterilization generally uses oxidizing process and ultraviolet method.However, chlorine or ozonization can produce sterilization by-product
Thing, trigger secondary pollution risk；Ultraviolet-sterilization is higher to equipment requirement, and energy consumption is big.Research shows, at least containing eight carbon
The bactericidal property, relatively low bacteriocidal concentration, lasting sterilization that the quarternary ammonium salt compound of atom above carbochain has broad-spectrum high efficacy are imitated
The various features such as fruit and safety and low toxicity, are received significant attention.Quarternary ammonium salt compound belongs to non-oxidative bactericide, will not produce and disappear
Toxic byproduct, and cheap, it is low for equipment requirements, energy consumption is small, there is unique advantage in water sterilization.Small molecule quaternary ammonium
Salt is soluble in water, easy to foaming and can not reuse, thus need to be made into water-insoluble support type quaternary ammonium salt bactericide with gram
Disadvantages mentioned above is taken, while can be reused after regenerating；Further, since there is higher charge density after load, because
This has more preferable bactericidal property than small molecule quaternary ammonium salt.
At present, common immobilization technology is that quaternary ammonium salt bactericide is fixed in polymer resin matrix, such as the tree of nylon 6
Fat and cationic ion-exchange resin etc..And a large amount of poisonous organic reagents are used in high-molecular organic material synthesis, complex process, into
This is higher, and produces poisonous intermediate by-products, causes secondary pollution serious.
The content of the invention
The invention aims to solve defect present in prior art, there is provided and one kind has efficient sterilizing performance,
Cost is low, and environment amenable bactericide.
In order to achieve the above object, the invention provides a kind of biological material for solidifying quaternary ammonium salt, the biological material
Surface cure has quaternary ammonium salt；The chemical formula of quaternary ammonium group is：−N+R (CH3)2, wherein, R C8H17、−C10H21、−C12H25、−
C14H29Or C16H33；The content of quaternary ammonium group is 0.1 ~ 1.5 mmol/g.
Wherein, biological material is using rice straw, wheat stalk, tea waste, peanut skin, giantreed, maize straw, big
Beanstalk stalk etc., particle size are 0.1 ~ 2 mm.
Preferably, biological material uses wheat stalk or maize straw, the chemistry of the long chain quaternary ammonium group of surface cure
Formula is N+ C12H25 (CH3) 2）Or N+ C14H29 (CH3) 2, content is 0.8 ~ 1.4 mmol/g.
Optimal, biological material uses wheat stalk, and the chemical formula of the long chain quaternary ammonium group of surface cure is N+
C12H25 (CH3) 2, content is 1.4 mmol/g.
Present invention also offers the preparation method of above-mentioned biological material, comprise the following steps：Take 0.5 ~ 15g particle diameters big
Small is 0.1 ~ 2 mm biological material, add 2 ~ 250 mL solvents, add the mL of epoxychloropropane 5 ~ 200, temperature be 30 ~
The h of stirring reaction 0.5 ~ 12 under the conditions of 110 DEG C；Then 2 ~ 300 mL aminated reagent is added, is stirred under the conditions of 30 ~ 110 DEG C
React 0.5 ~ 12 h；Solvent uses N-N dimethylformamides, N-N dimethyl acetamides, methanol, acetone or toluene；Aminated examination
Agent uses eight alkyl dimethyl tertiary amides, ten alkyl dimethyl tertiary amides, Dodecyl Dimethyl Amine or dodecyldimethylamine base uncle
Amine or hexadecyldimethyl benzyl ammonium tertiary amine.
Preferably, biological material uses wheat stalk or maize straw；Solvent is using N-N dimethylformamides, N-N bis-
Methylacetamide or methanol；The aminated reagent uses Dodecyl Dimethyl Amine or dodecyldimethylamine base tertiary amine.
Optimal, the preparation method of the biological material of above-mentioned solidification quaternary ammonium salt is as follows：It is 0.5-0.8 to take 5g particle sizes
Mm wheat stalk, 50 mL N-N dimethyl acetamides are added as solvent, the mL of epoxychloropropane 50 is added, is in temperature
The h of stirring reaction 2 under the conditions of 100 DEG C；Then 50 mL aminated reagent is added, the h of stirring reaction 3 under the conditions of 100 DEG C.
Present invention also offers application of the above-mentioned biological material in terms of water body disinfection processing.
For the biological material when for water body disinfection, regulation water pH value is 5 ~ 8, and input amount is 1 ~ 10 g/L.
Biological material carries out activating and regenerating after terminating for water body disinfection, using alkali salt solution；Alkali salt solution is
NaCl and NaOH mixed solution, the wherein molar concentration of Na ions are that 0.1-2 mol/L, NaCl and NaOH mol ratio are
0.1:1-10:1。
Specific activating and regenerating method is as follows：Used biological material is filtered out from water, is added to NaCl and NaOH
Mixed solution in, 25 DEG C ~ 60 DEG C vibration 2 ~ 24 h after filter out, material is washed till neutrality using pure water, then moistened with absolute ethyl alcohol
Wash 1 ~ 3 time, be placed in 30 DEG C ~ 60 DEG C vacuum drying chambers and dry 12 ~ 24h.
The present invention has advantages below compared with prior art：
（1）It is soluble in water, easy that the present invention using biomass-based immobilization quaternary ammonium salt as bactericide overcomes small molecule quaternary ammonium salt
The shortcomings that bubbling and can not reusing, and can be reused after regenerating.There is higher electric charge after immobilization
Density, therefore there is higher bactericidal property than small molecule quaternary ammonium salt.
（2）The present invention can both overcome existing sterilization material using agricultural wastes biological material as matrix simultaneously
Cost is too high and the problem of secondary pollution, can realize the recycling of agricultural wastes again, has certain social and economical
Value.
（3）The present invention prepares the immobilization quaternary ammonium salt bactericide using biomass as matrix, and preparation method is simple to operation, right
Environmental nonpollution, cost are cheap.
（4）The biological material that the present invention is prepared, it is expected to succinct, efficient realize to bacterium in water and pathogen
Deep purifying, the improvement of advanced treating and Polluted raw water for biochemical tail water provide new approaches, there is preferable novelty.
Brief description of the drawings
Fig. 1 is to solidify chemical equation prepared by the biological material of quaternary ammonium salt in the embodiment of the present invention 6；
Fig. 2 be the embodiment of the present invention 6 in be prepared solidification quaternary ammonium salt biological material to water body sterilization effect before and after
Comparison diagram.
In figure, before a is sterilizing, after b is sterilizing.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
The wheat stalk particle for taking 0.5 g to sieve（0.1~0.8 mm）Three-necked flask is put into, adds 2 mL N-N dimethyl formyls
Amine, another to add 5 mL epoxychloropropane, the h of stirring reaction 0.5 under the conditions of being 30 DEG C in temperature.Secondly, the alkyl of 10 mL eight is added
Dimethyl tertiary amine, 40 DEG C of h of stirring reaction 1, biomass-based immobilization quaternary ammonium salt bactericide 1 is made.
Wherein, the content of quaternary ammonium salt is 0.1 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>104Escherichia coli can completely be killed, reached by CFU/mL, 10 g/L materials 1
National drinking water standard.
Embodiment 2
The corn stalk pelletses for taking 2 g to sieve（0.2~0.6 mm）Three-necked flask is put into, adds 20 mL N-N dimethyl formyls
Amine, another to add 20 mL epoxychloropropane, the h of stirring reaction 1.5 under the conditions of being 40 DEG C in temperature.Secondly, the alkane of 20 mL ten is added
Base dimethyl tertiary amine, 50 DEG C of h of stirring reaction 1.5, biomass-based immobilization quaternary ammonium salt bactericide 2 is made.
Wherein, the content of quaternary ammonium salt is 0.15 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 5, E. CoIi content>105Escherichia coli can completely be killed, reached by CFU/mL, 5 g/L materials 2
National drinking water standard.
Embodiment 3
The wheat stalk particle for taking 5 g to sieve（0.5~0.8 mm）Three-necked flask is put into, adds 50 mL N-N dimethyl formyls
Amine, another to add 50 mL epoxychloropropane, the h of stirring reaction 2 under the conditions of being 60 DEG C in temperature.Secondly, 20 mL dodecanes are added
Base dimethyl tertiary amine, 60 DEG C of h of stirring reaction 2, biomass-based immobilization quaternary ammonium salt bactericide 3 is made.
Wherein, the content of quaternary ammonium salt is 0.3 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6.5, E. CoIi content>105Escherichia coli can completely be killed, reached by CFU/mL, 4 g/L materials 3
To national drinking water standard.
Embodiment 4
The wheat stalk particle for taking 10 g to sieve（0.8~1.5 mm）Three-necked flask is put into, adds 100 mL N-N dimethyl methyls
Acid amides, another to add 100 mL epoxychloropropane, the h of stirring reaction 4 under the conditions of being 80 DEG C in temperature.Secondly, 220 mL 14 are added
Alkyl dimethyl tertiary amide, 80 DEG C of h of stirring reaction 4, biomass-based immobilization quaternary ammonium salt bactericide 4 is made.
Wherein, the content of quaternary ammonium salt is 0.5 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 7, E. CoIi content>106Escherichia coli can completely be killed, reached by CFU/mL, 2.5 g/L materials 4
To national drinking water standard.
Embodiment 5
The wheat stalk particle for taking 15 g to sieve（1~2 mm）Three-necked flask is put into, adds 250 mL N-N dimethylformamides,
It is another to add 200 mL epoxychloropropane, the h of stirring reaction 12 under the conditions of being 100 DEG C in temperature.Secondly, 300 mL hexadecanes are added
Base dimethyl tertiary amine, 100 DEG C of h of stirring reaction 12, biomass-based immobilization quaternary ammonium salt bactericide 5 is made.
Wherein, the content of quaternary ammonium salt is 0.9 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>106Escherichia coli can completely be killed, reached by CFU/mL, 2 g/L materials 5
National drinking water standard.
Embodiment 6
The wheat stalk particle for taking 5 g to sieve（0.5~1 mm）Three-necked flask is put into, adds 50 mL N-N dimethylformamides,
It is another to add 100 mL epoxychloropropane, the h of stirring reaction 2 under the conditions of being 100 DEG C in temperature.Secondly, 100 mL dodecyls are added
Dimethyl tertiary amine, 100 DEG C of stirring reaction 3h, biomass-based immobilization quaternary ammonium salt bactericide 6 is made, as shown in Figure 1.
Wherein, the quality for the bactericide 1 being prepared is 5.8 g, and the content of quaternary ammonium salt is 1.4 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 7, E. CoIi content>107CFU/mL, 1g/L material 6 can kill Escherichia coli completely（Such as Fig. 2
It is shown）, reach national drinking water standard.
Embodiment 7
The maize straw for taking 6 g to sieve（0.5~1mm）Three-necked flask is put into, adds 60 mL N-N dimethylformamides, it is another to add
120 mL epoxychloropropane, stirring reaction 2h under the conditions of being 95 DEG C in temperature.Secondly, 120 mL hexadecyldimethyl benzyl ammonium uncles are added
Amine, 95 DEG C of stirring reaction 4h, biomass-based immobilization quaternary ammonium salt bactericide 7 is made.
Wherein, the content of quaternary ammonium salt is 1.3 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6.5, E. CoIi content>106CFU/mL, 1g/L material 7 can kill Escherichia coli completely, reach
National drinking water standard.
Embodiment 8
The rice straw for taking 2.5 g to sieve（0.5~1.2 mm）Three-necked flask is put into, adds 100 mL N-N dimethylformamides,
It is another to add 100 mL epoxychloropropane, the h of stirring reaction 2 under the conditions of being 90 DEG C in temperature.Then 100 mL dodecyls two are added
Methyl tertiary amine, 90 DEG C of stirring reaction 3h, biomass-based immobilization quaternary ammonium salt bactericide 8 is made.
Wherein, the content of quaternary ammonium salt is 1.1 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 8, E. CoIi content>106Escherichia coli can completely be killed, reached by CFU/mL, 1.8 g/L materials 8
To national drinking water standard.
Embodiment 9
The tea waste for taking 0.5g to sieve（0.2~0.4mm）Three-necked flask is put into, adds 30mL N-N dimethylformamides, it is another to add
Enter 20mL epoxychloropropane, the h of stirring reaction 0.5 under the conditions of being 85 DEG C in temperature.Secondly, the alkyl dimethyls of 20 mL eight are added
Tertiary amine, 85 DEG C of h of stirring reaction 0.5, biomass-based immobilization quaternary ammonium salt bactericide 9 is made.
Wherein, the content of quaternary ammonium salt is 0.7 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>5×105CFU/mL, 5g/L material 9 can kill Escherichia coli completely, reach
To national drinking water standard.
Embodiment 10
The peanut skin for taking 3 g to sieve（0.8~1.5 mm）Three-necked flask is put into, adds 100 mL N-N dimethylformamides, it is another to add
Enter 80 mL epoxychloropropane, stirring reaction 6h under the conditions of being 75 DEG C in temperature.Secondly, 80 mL dodecyl dimethyl uncles are added
Amine, 75 DEG C of stirring reaction 6h, biomass-based immobilization quaternary ammonium salt bactericide 10 is made.
Wherein, the content of quaternary ammonium salt is 1.0 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>107CFU/mL, 1.5g/L material 10 can kill Escherichia coli completely, reach
To national drinking water standard.
Embodiment 11
The giantreed for taking 8 g to sieve（1~2 mm）The three-necked flask that is put into of drying is cleaned, adds 150 mL N-N dimethylformamides,
It is another to add 100 mL epoxychloropropane, stirring reaction 8h under the conditions of being 110 DEG C in temperature.Secondly, 100 mL myristyls are added
Dimethyl tertiary amine, 110 DEG C of stirring reaction 8h, biomass-based immobilization quaternary ammonium salt bactericide 11 is made.
Wherein, the content of quaternary ammonium salt is 0.8 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>106 Escherichia coli can completely be killed, reached by CFU/mL, 2 g/L materials 11
National drinking water standard.
Embodiment 12
The maize straw for taking 10 g to sieve（2~3mm）Three-necked flask is put into, adds 200 mL N-N dimethylformamides, it is another to add
150 mL epoxychloropropane, stirring reaction 6h under the conditions of being 100 DEG C in temperature.Secondly, 150 mL hexadecyldimethyl benzyl ammoniums are added
Tertiary amine, 100 DEG C of stirring reaction 6h, biomass-based immobilization quaternary ammonium salt bactericide 12 is made.
Wherein, the content of quaternary ammonium salt is 0.9 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>106CFU/mL, 2g/L material 12 can kill Escherichia coli completely, reach
National drinking water standard.
Embodiment 13
The soybean stalk for taking 10 g to sieve（1~2mm）Three-necked flask is put into, adds 300mL N-N dimethylformamides, it is another to add
200mL epoxychloropropane, stirring reaction 8h under the conditions of being 110 DEG C in temperature.Secondly, 200mL dodecyl dimethyl uncles are added
Amine, 110 DEG C of h of stirring reaction 8, biomass-based immobilization quaternary ammonium salt bactericide 13 is made.
Wherein, the content of quaternary ammonium salt is 0.6 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>106 Escherichia coli can completely be killed, reached by CFU/mL, 3 g/L materials 13
National drinking water standard.
Embodiment 14
The rice straw for taking 15 g to sieve（0.8~1mm）Three-necked flask is put into, adds 500mL N-N dimethylformamides, it is another to add
Enter 200mL epoxychloropropane, the h of stirring reaction 12 under the conditions of being 65 DEG C in temperature.Secondly, 200mL dimethyls are added
Base tertiary amine, 65 DEG C of stirring reaction 12h, biomass-based immobilization quaternary ammonium salt bactericide 14 is made.
Wherein, the content of quaternary ammonium salt is 0.5 mmol/g.
Experiment shows that biomass-based immobilization quaternary ammonium salt bactericide obtained above has obvious remove to bacterium in water
Effect.When pH value of solution be 6, E. CoIi content>106Escherichia coli can completely be killed, reached by CFU/mL, 1.5 g/L materials 14
To national drinking water standard.
Claims (10)
- A kind of 1. biological material for solidifying quaternary ammonium salt, it is characterised in that：The biological material surface cure has long chain quaternary ammonium Group；The chemical formula of the long chain quaternary ammonium group is：−N+R (CH3)2, wherein, R C8H17、−C10H21、−C12H25、−C14H29 Or C16H33；The content of the quaternary ammonium group is 0.1 ~ 1.5 mmol/g.
- 2. biological material according to claim 1, it is characterised in that：The biological material is using rice straw, small Wheat Straw, tea waste, peanut skin, giantreed, maize straw, soybean stalk etc., particle size are 0.1 ~ 2 mm.
- 3. biological material according to claim 2, it is characterised in that：The biological material uses wheat stalk or jade Rice stalk, the chemical formula of the long chain quaternary ammonium group of surface cure is N+ C12H25 (CH3) 2）Or N+ C14H29 (CH3) 2, Content is 0.8 ~ 1.4 mmol/g.
- 4. biological material according to claim 3, it is characterised in that：The biological material uses wheat stalk, table The chemical formula of the long chain quaternary ammonium group of face solidification is N+ C12H25 (CH3) 2, content is 1.4 mmol/g.
- 5. the preparation method of the biological material of claim 1 or 2, it is characterised in that：Comprise the following steps：Take 0.5 ~ 15 g Particle diameter is 0.1 ~ 2 mm biological material, adds 2 ~ 250 mL solvents, adds the mL of epoxychloropropane 5 ~ 200, is 30 in temperature The h of stirring reaction 0.5 ~ 12 under the conditions of ~ 110 DEG C；Then 2 ~ 300 mL aminated reagent is added, is stirred under the conditions of 30 ~ 110 DEG C React 0.5 ~ 12 h；The solvent uses N-N dimethylformamides, N-N dimethyl acetamides, methanol, acetone or toluene；It is described Aminated reagent is using eight alkyl dimethyl tertiary amides, ten alkyl dimethyl tertiary amides, Dodecyl Dimethyl Amine, myristyl two Methyl tertiary amine or hexadecyldimethyl benzyl ammonium tertiary amine.
- 6. preparation method according to claim 5, it is characterised in that：The biological material uses wheat stalk or corn Stalk；The solvent uses N-N dimethylformamides, N-N dimethyl acetamides or methanol；The aminated reagent uses 12 Alkyl dimethyl tertiary amide, dodecyldimethylamine base tertiary amine.
- 7. preparation method according to claim 6, it is characterised in that：Comprise the following steps：Take 5 g particle sizes for 0.5 ~ 1 mm wheat stalk, 50 mL N-N dimethyl acetamides are added as solvent, the mL of epoxychloropropane 50 is added, is in temperature The h of stirring reaction 2 under the conditions of 100 DEG C；Then 50 mL aminated reagent Dodecyl Dimethyl Amine, 100 DEG C of conditions are added The lower h of stirring reaction 3.
- 8. application of any biological material of Claims 1-4 in terms of water body disinfection processing.
- 9. application according to claim 8, it is characterised in that：The biological material is when for water body disinfection, input Measure as 1 ~ 10 g/L.
- 10. application according to claim 9, it is characterised in that：The biological material after terminating for water body disinfection, Activating and regenerating is carried out using alkali salt solution；The alkali salt solution is mole of NaCl and NaOH mixed solution, wherein Na ions Concentration is that 0.1 ~ 2 mol/L, NaCl and NaOH mol ratio are 0.1:1~10:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710945437.6A CN107668034A (en) | 2017-10-12 | 2017-10-12 | A kind of biological material for solidifying quaternary ammonium salt and preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710945437.6A CN107668034A (en) | 2017-10-12 | 2017-10-12 | A kind of biological material for solidifying quaternary ammonium salt and preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107668034A true CN107668034A (en) | 2018-02-09 |
Family
ID=61140529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710945437.6A Pending CN107668034A (en) | 2017-10-12 | 2017-10-12 | A kind of biological material for solidifying quaternary ammonium salt and preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107668034A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113210023A (en) * | 2021-04-29 | 2021-08-06 | 黄山学院 | Biochar-based anion exchanger and preparation method and application thereof |
| CN115918655A (en) * | 2022-03-18 | 2023-04-07 | 中国矿业大学(北京) | Modified porous material, preparation method thereof and application of modified porous material in killing bacteria/fungi and inactivating viruses in water body |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101091906A (en) * | 2007-06-13 | 2007-12-26 | 山东大学 | Cationoid adsorbent for quarternary ammonium salt of agricultural waste, and preparation technique |
| CN101342485A (en) * | 2008-07-03 | 2009-01-14 | 山东大学 | Method for preparing quaternary amines salt cationic adsorption agent with plant of high cellulose content |
| CN101721978A (en) * | 2009-12-18 | 2010-06-09 | 华东理工大学 | Adsorbent for polyaromatic hydrocarbon pollutant, preparation method and application thereof |
| CN102764635A (en) * | 2012-08-10 | 2012-11-07 | 广西师范大学 | Method for preparing quaternary ammonium salt cationic absorbing agent by using manioc straw/ manioc waste and application |
| CN103340202A (en) * | 2013-06-03 | 2013-10-09 | 山东省泰和水处理有限公司 | Preparation method for high-efficiency oilfield bactericide |
| CN104353440A (en) * | 2014-11-28 | 2015-02-18 | 南京信息工程大学 | Biomass resin based inorganic nano-oxide composite adsorbent and preparation method and application thereof |
| CN105214629A (en) * | 2015-10-30 | 2016-01-06 | 南京信息工程大学 | A kind of biomass-based nano lanthanum oxide dephosphorization compound adsorbent and preparation method thereof |
| CN106219657A (en) * | 2016-08-01 | 2016-12-14 | 华南理工大学 | A kind of modified biomass adsorbent and its preparation method and application |
-
2017
- 2017-10-12 CN CN201710945437.6A patent/CN107668034A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101091906A (en) * | 2007-06-13 | 2007-12-26 | 山东大学 | Cationoid adsorbent for quarternary ammonium salt of agricultural waste, and preparation technique |
| CN101342485A (en) * | 2008-07-03 | 2009-01-14 | 山东大学 | Method for preparing quaternary amines salt cationic adsorption agent with plant of high cellulose content |
| CN101721978A (en) * | 2009-12-18 | 2010-06-09 | 华东理工大学 | Adsorbent for polyaromatic hydrocarbon pollutant, preparation method and application thereof |
| CN102764635A (en) * | 2012-08-10 | 2012-11-07 | 广西师范大学 | Method for preparing quaternary ammonium salt cationic absorbing agent by using manioc straw/ manioc waste and application |
| CN103340202A (en) * | 2013-06-03 | 2013-10-09 | 山东省泰和水处理有限公司 | Preparation method for high-efficiency oilfield bactericide |
| CN104353440A (en) * | 2014-11-28 | 2015-02-18 | 南京信息工程大学 | Biomass resin based inorganic nano-oxide composite adsorbent and preparation method and application thereof |
| CN105214629A (en) * | 2015-10-30 | 2016-01-06 | 南京信息工程大学 | A kind of biomass-based nano lanthanum oxide dephosphorization compound adsorbent and preparation method thereof |
| CN106219657A (en) * | 2016-08-01 | 2016-12-14 | 华南理工大学 | A kind of modified biomass adsorbent and its preparation method and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113210023A (en) * | 2021-04-29 | 2021-08-06 | 黄山学院 | Biochar-based anion exchanger and preparation method and application thereof |
| CN115918655A (en) * | 2022-03-18 | 2023-04-07 | 中国矿业大学(北京) | Modified porous material, preparation method thereof and application of modified porous material in killing bacteria/fungi and inactivating viruses in water body |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108339526B (en) | Modified sodium alginate adsorption material for adsorbing tetracycline antibiotics and preparation method thereof | |
| CN104370333B (en) | The preparation method of the active reverse-phase emulsifier of a kind of strong interface | |
| CN106006998A (en) | Attapulgite/denitrifier composite type wastewater treating agent and preparation method thereof | |
| CN101305733B (en) | Water-insoluble phosphonium salt bactericidal agent and its preparation method | |
| CN107668034A (en) | A kind of biological material for solidifying quaternary ammonium salt and preparation method and application | |
| CN107570191A (en) | A kind of Preparation method and use of visible light catalyst | |
| CN101880084A (en) | Preparation method of novel biological denitrification controlled release carbon source carriers | |
| CN105543150B (en) | Bioremediation preparation for aniline polluted water | |
| CN103880991B (en) | A kind of have antibacterial macromolecule polymer material with trace-element slow-release function and preparation method thereof | |
| CN107129582B (en) | Arborization sterilization microsphere and preparation method and application thereof | |
| CN107469772A (en) | A kind of method of heavy metal classes incretion interferent in removal reverse osmosis concentrated water | |
| CN102784623B (en) | Preparation method of non-dissolving antibacterial polyquaternium modified active carbon | |
| CN107099483A (en) | A kind of composite biological agent and its application in processing mercury-containing waste water | |
| CN105731653B (en) | Handle the preparation and processing method of aniline waste water | |
| CN102924723B (en) | Insoluble polymeric quaternary ammonium salt bactericide, preparation method thereof and sterilization packed bed | |
| CN106745450A (en) | A kind of adsorption treatment method of Ciprofloxacin in sewage | |
| CN107011467B (en) | A kind of functionalization sterilization microballoon and its preparation method and application | |
| CN1165226C (en) | Water insoluble germicide and its preparation | |
| CN109179615A (en) | A kind of modified cotton fiber coagulant and its preparation method and application | |
| CN107022077B (en) | Chlorine ball is grafted the method and its application of dendrimer preparation immobilization fungicide | |
| CN1086914C (en) | Water insoluble polyquaternary phosphonium salt germicide | |
| CN107570122A (en) | A kind of difunctional hybrid material of biomass and preparation method and application | |
| CN1128577C (en) | Polymer-type amphoteric disinfectant and its preparing process | |
| CN1128578C (en) | Polymer-type amphoteric disinfectant and its preparing process | |
| CN109499549A (en) | A kind of mercury ion absorption sponge and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 210044 No. 219 Ning six road, Jiangbei new district, Nanjing, Jiangsu Applicant after: Nanjing University of Information Science and Technology Address before: No. 69, Jianye District, Jianye District, Nanjing, Jiangsu Applicant before: Nanjing University of Information Science and Technology |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180209 |