CN109651281A - A kind of melamine bismuth complex raw powder's production technology and its application - Google Patents

A kind of melamine bismuth complex raw powder's production technology and its application Download PDF

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CN109651281A
CN109651281A CN201811555320.8A CN201811555320A CN109651281A CN 109651281 A CN109651281 A CN 109651281A CN 201811555320 A CN201811555320 A CN 201811555320A CN 109651281 A CN109651281 A CN 109651281A
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melamine
bismuth
powder
application
sewage
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CN109651281B (en
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韩成良
沈寿国
朱聪
徐泽忠
姚李
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Hebei Shengchuangxin Materials Co ltd
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Hefei University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D251/00Heterocyclic compounds containing 1,3,5-triazine rings
    • C07D251/02Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
    • C07D251/12Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
    • C07D251/26Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
    • C07D251/40Nitrogen atoms
    • C07D251/54Three nitrogen atoms
    • C07D251/56Preparation of melamine
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/16Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/18Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
    • B01J31/1805Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
    • B01J31/181Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
    • B01J31/1815Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine with more than one complexing nitrogen atom, e.g. bipyridyl, 2-aminopyridine
    • 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
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • 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
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5272Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using specific organic precipitants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2531/00Additional information regarding catalytic systems classified in B01J31/00
    • B01J2531/50Complexes comprising metals of Group V (VA or VB) as the central metal
    • B01J2531/54Bismuth
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates
    • 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
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • 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
    • C02F2101/38Organic compounds containing nitrogen
    • 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
    • C02F2101/40Organic compounds containing sulfur
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

A kind of melamine bismuth complex raw powder's production technology and its application are related to complex material preparation and technical field of sewage.First by (Bi (NO3)3·5H2O it) is dissolved in deionized water and is configured to aqueous bismuth nitrate solution;Then at room temperature, by melamine (C3N3(NH2)3) be added into aqueous bismuth nitrate solution, it can be obtained melamine bismuth cooperation powder after ultrasonic dissolution and complexation reaction.The present invention can obtain such as rodlike, band-like, sheet and plate-like melamine bismuth complex using different amounts of melamine, to realize the controllable preparation of variform melamine bismuth cooperation powder.The melamine bismuth cooperation powder of preparation have well can the melamine bismuth of absorbing properties and heavy metal paved set ability cooperate powder, each pollutant in aqueous systems can be effectively removed, it is expected to as sewage treatment new material.

Description

A kind of melamine bismuth complex raw powder's production technology and its application
Technical field
The present invention relates to complex material preparation and technical field of sewage, are specifically related to a kind of melamine bismuth Complex raw powder's production technology and its application.
Background technique
Melamine (C3N6H6, L) and it is a kind of triazines nitrogen heterocyclic ring organic compound, it is pure white monoclinic prism body, is in Alkalescent (pKb=8), can form melamine salt in an acidic solution.Single C3N6H6Molecule is by a carbon nitrogen aromatic rings and three A amino composition.In relation to melamine (L) and bivalent metal ion (M2+)(M2+It can be Ca2+、Mg2+、Zn2+、Cu2+、Ni2+) formed Melamine metal complex ML2(OH)2It studies and reports and is more.
In general, aqueous bismuth nitrate solution is in stronger acidity, and melamine alkalescent, the two can occur acid-base neutralization and Complexation reaction provides new idea and method to obtain melamine bismuth complex.The present invention exactly with melamine be with Body, at normal temperature by with Bi3+Complexation reaction occurs, melamine bismuth cooperation powder has successfully been obtained, it is expected to be used as at sewage Reason uses new material.
Summary of the invention
The present invention provides a kind of melamine for having the shortcoming prepared in the presence of melamine metal complex Amine bismuth complex raw powder's production technology and its application.
To achieve the goals above, the technical scheme adopted by the invention is as follows: a kind of melamine bismuth cooperation powder Preparation method, steps are as follows: first by (Bi (NO3)3·5H2O it) is dissolved in deionized water and is configured to aqueous bismuth nitrate solution;Then exist At room temperature, by melamine (C3N3(NH2)3) be added into aqueous bismuth nitrate solution, it can be obtained after ultrasonic dissolution and complexation reaction It obtains melamine bismuth and cooperates powder.
As the optimal technical scheme of preparation method of the present invention, the concentration of the aqueous bismuth nitrate solution is 5~15g/L, often The additive amount of melamine is 1~30g in 1L aqueous bismuth nitrate solution.The temperature of the complexation reaction is room temperature, reaction time 2 ~10min.
The present invention also provides a kind of applications of melamine bismuth cooperation powder, and melamine bismuth cooperation powder is thrown It is put into containing Cr2O7 2-Or Cu2+Sewage in, pass through complex-precipitation reaction and remove dirty water pollutant.Alternatively, by melamine bismuth Cooperate powder to launch into the sewage containing organic dyestuff, dirty water pollutant is removed by visible light photocatalytic degradation.There is engine dyeing Material is rhodamine B, methylene blue and methyl orange.The treatment temperature that visible light photocatalytic degradation removes organic dyestuff in sewage is room Temperature, it is seen that radiant is common sunlight.
As the optimal technical scheme of melamine bismuth complex powder application of the present invention, the melamine bismuth of dispensing cooperates Cr in powder and sewage2O7 2-Or Cu2+Molar ratio be 1~3:1.Alternatively, to 100mL organic dyestuff concentration be 10mg/L 0.2~1g melamine bismuth is launched in sewage cooperates powder.
Compared with prior art, beneficial effects of the present invention are shown:
1), the present invention passes through melamine and Bi using melamine as ligand at normal temperature3+Complexation reaction occurs successfully to obtain Melamine bismuth cooperation powder was obtained, meanwhile, such as rodlike, band-like, sheet can be obtained using different amounts of melamine With plate-like melamine bismuth complex, thus realize variform melamine bismuth cooperation powder controllable preparation.
2), the present invention using melamine as ligand, have successfully been obtained at normal temperatures and pressures have well can absorbing properties Cooperate powder with the melamine bismuth of heavy metal paved set ability, each pollutant in aqueous systems can be effectively removed, it is expected to As sewage treatment new material.
3), preparation method of the invention has the characteristics that easy to operate, low in cost, acquisition product amount is big, cooperates for bismuth The preparation and application of powder provide new approaches and frontier.
Detailed description of the invention
Fig. 1 is the form and chemical composition for preparing product in embodiment 1 when melamine additive amount is 0.1g;
Fig. 2 is the form and chemical composition for preparing product in embodiment 1 when melamine additive amount is 1g;
Fig. 3 is the form and chemical composition for preparing product in embodiment 1 when melamine additive amount is 1.5g;
Fig. 4 is the form and chemical composition for preparing product in embodiment 1 when melamine additive amount is 3g;
Fig. 5 a is the visible absorption spectrum that melamine bismuth cooperates powder, and Fig. 5 b is melamine bismuth in embodiment 3 Cooperate the photocatalytic degradation curve of organic dyestuff rhodamine B in powder removal sewage.
Specific embodiment
With reference to embodiments with attached drawing to melamine bismuth complex raw powder's production technology of the invention and its application It makes and being discussed further.Flied emission scanning electron microscopy is respectively adopted in structure, the form performance of the method for the present invention products therefrom Mirror (FE-SEM, SU8010) and ultraviolet-visible spectrometer (Vb300) are characterized and are analyzed.
Embodiment 1
Melamine bismuth cooperates the preparation of powder, and steps are as follows:
It is divided into four groups of experiments, first by the (Bi (NO of 0.5g in every group of experiment3)3·5H2O) it is dissolved in the deionized water of 100mL In be configured to aqueous bismuth nitrate solution.
Then, at room temperature, respectively by the melamine (C of 0.1g, 1g, 1.5g, 3g3N3(NH2)3) be added to bismuth nitrate It, can product after ultrasonic dissolution and complexation reaction 5min in aqueous solution.
Fig. 1~4 are respectively the shape for preparing product in embodiment 1 when melamine additive amount is 0.1g, 1g, 1.5g, 3g State and chemical composition can obtain such as rodlike (Fig. 1), band-like using different amounts of melamine as seen in Figure 1 The melamine bismuth complex of (Fig. 2), sheet (Fig. 3) and plate-like (Fig. 4) different shape.
The formation of melamine bismuth complex can be regarded as by following two process: firstly, melamine hydrolyzes Reaction generates L (OH)3;Then, L (OH)3With Bi3+Form BiL3(OH)3, above-mentioned two process can use formula (1) and (2) It respectively indicates:
Embodiment 2
Melamine bismuth cooperates the mechanism of chromium and copper in powder removing waste water
Weigh melamine bismuth complex dry powder (preparation production when melamine additive amount is 1.5g in embodiment 1 of 0.5g Object) it is respectively put into certain density Cr2O7 2-And Cu2+(melamine bismuth cooperates Cr in powder and sewage to waste water2O7 2-Or Cu2+ Molar ratio be 1:1 or more, it is appropriate excessive best) in, can be removed in water body by real-time coordination and precipitation reaction Cr2O7 2-And Cu2+Etc. heavy metal ion.Complex removes Cr2O7 2-And Cu2+Mechanism such as formula (3) and (4) shown in.
Embodiment 3
Melamine bismuth cooperates powder to remove organic dyestuff in wastewater performance
Firstly, can detecte to obtain the visible absorption of melamine bismuth cooperation powder by ultraviolet-visible spectrometer Spectrum, as shown in Figure 5 a, it can be seen that visible-UV absorption maximum wavelength of product is about 480nm (see illustration).
It then, is 10mg/L with concentration, the rhodamine B aqueous solution that volume is 100mL is that target organic contamination source is object, It is separately added into the cooperation powder of 0.2g, 0.4g, ultrasonic disperse is protected from light processing after sixty minutes at room temperature, then is put under sunlight Irradiation 100 minutes, rhodamine B concentration (C in systemt) as shown in Figure 5 b with the relationship of irradiation time (t).With catalyst feelings are not added Comparison can be seen that the extension with sunlight irradiation time under condition, and the amount of rhodamine B is gradually decreasing in system, and explanation is matched Closing object has good visible light catalytic performance.And in system for handling be added 0.4g cooperation powder treatment effect be better than plus Enter 0.2g cooperation powder, addition 0.4g cooperation powder irradiates 100 minutes under sunlight can completely remove Luo Dan substantially Bright B.
Embodiment 4
Melamine bismuth cooperates the preparation of powder, and steps are as follows:
First by the (Bi (NO of 1g3)3·5H2O it) is dissolved in the deionized water of 100mL and is configured to aqueous bismuth nitrate solution;It connects , at room temperature, respectively by the melamine (C of 1g3N3(NH2)3) be added into aqueous bismuth nitrate solution, through ultrasonic dissolution and match Position reaction 2min after can product, product be melamine bismuth cooperation powder.
Embodiment 5
Melamine bismuth cooperates the preparation of powder, and steps are as follows:
First by the (Bi (NO of 1.5g3)3·5H2O it) is dissolved in the deionized water of 100mL and is configured to aqueous bismuth nitrate solution;It connects , at room temperature, respectively by the melamine (C of 3g3N3(NH2)3) be added into aqueous bismuth nitrate solution, through ultrasonic dissolution and match Position reaction 10min after can product, product be melamine bismuth cooperation powder.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention Design or beyond the scope defined by this claim, be within the scope of protection of the invention.

Claims (10)

1. a kind of melamine bismuth complex raw powder's production technology, which is characterized in that steps are as follows: first by (Bi (NO3)3· 5H2O it) is dissolved in deionized water and is configured to aqueous bismuth nitrate solution;Then at room temperature, by melamine (C3N3(NH2)3) be added to nitre In sour bismuth aqueous solution, melamine bismuth cooperation powder can be obtained after ultrasonic dissolution and complexation reaction.
2. preparation method as described in claim 1, which is characterized in that the concentration of the aqueous bismuth nitrate solution is 5~15g/L, The additive amount of melamine is 1~30g in every 1L aqueous bismuth nitrate solution.
3. preparation method as described in claim 1, which is characterized in that the temperature of the complexation reaction is room temperature, reaction time For 2~10min.
4. a kind of melamine bismuth such as the method preparation of any one of claims 1 to 3 cooperates the application of powder, feature It is, melamine bismuth cooperation powder is launched to containing Cr2O7 2-Or Cu2+Sewage in, go to decontaminate by complex-precipitation reaction Water pollutant.
5. application as claimed in claim 4, which is characterized in that in the melamine bismuth cooperation powder and sewage of dispensing Cr2O7 2-Or Cu2+Molar ratio be 1~3:1.
6. a kind of melamine bismuth such as the method preparation of any one of claims 1 to 3 cooperates the application of powder, feature It is, melamine bismuth cooperation powder is launched into the sewage containing organic dyestuff, goes to decontaminate by visible light photocatalytic degradation Water pollutant.
7. application as claimed in claim 6, which is characterized in that thrown into the sewage that 100mL organic dyestuff concentration is 10mg/L Put 0.2~1g melamine bismuth cooperation powder.
8. application as claimed in claim 6, which is characterized in that visible light photocatalytic degradation removes the processing of organic dyestuff in sewage Temperature is room temperature.
9. application as claimed in claim 6, which is characterized in that visible light source is common sunlight.
10. application as claimed in claim 6, which is characterized in that organic dyestuff is rhodamine B, methylene blue and methyl orange.
CN201811555320.8A 2018-12-18 2018-12-18 Preparation method and application of melamine bismuth complex powder Active CN109651281B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106732735A (en) * 2017-01-18 2017-05-31 常州大学 A kind of composite of photocatalytic degradation Microcystin and preparation method and application
CN107626335A (en) * 2017-09-21 2018-01-26 浙江工商大学 A kind of bismuth system/carbonitride composite catalyst and its preparation method and application

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106732735A (en) * 2017-01-18 2017-05-31 常州大学 A kind of composite of photocatalytic degradation Microcystin and preparation method and application
CN107626335A (en) * 2017-09-21 2018-01-26 浙江工商大学 A kind of bismuth system/carbonitride composite catalyst and its preparation method and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
L. COSTA ET. AL.: "Thermal degradation and fire retardancy of animony and bismuth trihalides-melamine complexes", 《POLYMER DEGRADATION AND STABILITY》 *

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