CN109847785A - A kind of preparation method nitrogenizing carbon colloid - Google Patents
A kind of preparation method nitrogenizing carbon colloid Download PDFInfo
- Publication number
- CN109847785A CN109847785A CN201910138693.3A CN201910138693A CN109847785A CN 109847785 A CN109847785 A CN 109847785A CN 201910138693 A CN201910138693 A CN 201910138693A CN 109847785 A CN109847785 A CN 109847785A
- Authority
- CN
- China
- Prior art keywords
- preparation
- sulfur
- nitridation carbon
- hydrocarbons
- colloid
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 72
- 239000000084 colloidal system Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000000502 dialysis Methods 0.000 claims abstract description 33
- 239000000428 dust Substances 0.000 claims abstract description 32
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 32
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 29
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 238000013019 agitation Methods 0.000 claims abstract description 18
- 239000000320 mechanical mixture Substances 0.000 claims abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 30
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 30
- 229910052717 sulfur Chemical group 0.000 claims description 30
- 239000011593 sulfur Chemical group 0.000 claims description 30
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 4
- 229960000789 guanidine hydrochloride Drugs 0.000 claims description 3
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 35
- 239000000126 substance Substances 0.000 abstract description 28
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 24
- 239000002537 cosmetic Substances 0.000 abstract description 18
- 239000002689 soil Substances 0.000 abstract description 18
- 230000007613 environmental effect Effects 0.000 abstract description 15
- 239000004909 Moisturizer Substances 0.000 abstract description 9
- 230000000845 anti-microbial effect Effects 0.000 abstract description 9
- 238000004140 cleaning Methods 0.000 abstract description 9
- 230000001333 moisturizer Effects 0.000 abstract description 9
- 230000003020 moisturizing effect Effects 0.000 abstract description 9
- 239000010865 sewage Substances 0.000 abstract description 9
- 239000012620 biological material Substances 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 8
- 230000008635 plant growth Effects 0.000 abstract description 8
- 238000005067 remediation Methods 0.000 abstract description 8
- 239000000516 sunscreening agent Substances 0.000 abstract description 7
- 230000006378 damage Effects 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 15
- 239000000725 suspension Substances 0.000 description 14
- 238000007146 photocatalysis Methods 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 7
- 239000000499 gel Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000004964 aerogel Substances 0.000 description 6
- -1 moisture saver mask Substances 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 239000000017 hydrogel Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 125000004354 sulfur functional group Chemical group 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 238000000366 colloid method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000004815 dispersion polymer Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Colloid Chemistry (AREA)
Abstract
The present invention relates to catalysis material technical field more particularly to a kind of preparation methods for nitrogenizing carbon colloid.It include: addition hydrocarbons and the uniform ball milling formation compound particles of mechanical mixture into nitridation carbon dust；By the method for ultrasonic agitation, dialysis removes unreacted hydrocarbons after dissolving mixt particle, obtains nitridation carbon colloid.The preparation method of the embodiment of the present invention has yield high, concentration is big, the advantages of convenient for regulation and simple process, it can be applied to large-scale industrial production, applied to chemical industry, daily use chemicals, it is medical, the environmental protection in the fields such as agricultural and antimicrobial product, applied to air cleaning, sewage treatment, the chemical fields such as water body antibacterial, moisturizing cosmetic, moisture saver mask, the cosmetics such as suncream, medical antibacterial, the biomaterial for medical purpose such as Wound protection, soil remediation, water and soil moisturizer, soilless cultivation, the agricultural application such as plant growth, gel material is prepared by ep-type material, it can be avoided the harm for environment, and play Environmental Role.
Description
Technical field
The present invention relates to catalysis material technical field more particularly to a kind of preparation methods for nitrogenizing carbon colloid.
Background technique
Due to haze weather increasingly severe in recent years, so that air pollution problems inherent starts to receive more and more widely
Concern becomes the discussion hot spot of society.
In existing numerous air pollution processing technique, it is driving with solar energy, has the characteristics that the light of cleanliness without any pollution
Catalysis technique is to be presently considered to most possibly thoroughly solve the problems, such as one of preferred plan of FUTURE ENVIRONMENT.And wherein, development is high
Effect environmental protection and can large-scale practical application catalysis material be the photocatalysis technology field one of focus on research direction.
Traditional photocatalysis material of titanium dioxide receives its large-scale application seriously due to there was only ultraviolet light response
Limitation.Although Recent study personnel expand its activity under visible light conditions all the time.But due to technology and
Cost etc. the limitations of factors make it always and cannot reach the other requirement of technical grade.Therefore, develop visible-light photocatalysis material, from
It is the key breakthrough points that current photocatalysis technology moves towards application that cost, which meets industrial requirements with active angle,.
Carbonitride catalysis material is a kind of polymer semiconductor, because of its special characteristic of semiconductor (forbidden bandwidth Eg=
2.7eV), to have excellent visible light catalytic performance, good photochemical stability and higher thermal stability.In addition,
Due to its nonmetallic characteristic, it is nontoxic, low in cost the advantages that, photochemistry storage, environmental photochemistry administer, photocatalytic water system
The fields such as hydrogen energy storage have research extensively, are one of the materials for most having large-scale application prospect at present.
At the same time, the research of the various industrial scale applications of carbon nitride material is also continuously emerged, however it is main at present
And one of be most difficult to the direction broken through and be how for powdered carbon nitride material to be uniformly effectively dispersed in solvent, it makes
Standby is colloid or other kinds of dispersion, allows to easily coat and be fixed on corresponding daily life product
On, achieve the purpose that application.
In the implementation of the present invention, it is found by the applicant that following problem exists in the prior art: existing colloid preparation
In method, the method for strong acid protonation has biggish risk, and low yield, and the period is long, and economy and cost of labor are all difficult
To meet industrial requirements.Mechanical stripping rule focuses primarily upon the research of ultrasound removing, and efficiency is extremely low, is equally difficult to be applied
In industrial production.
Summary of the invention
Place in view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of preparation sides for nitrogenizing carbon colloid
Method, it is intended to which nitridation carbon colloid preparation efficiency is lower in the prior art for solution, and cost is excessively high, it is difficult to applied to actual industrial production
Problem.
In order to achieve the above object, first aspect of the embodiment of the present invention provides a kind of preparation method for nitrogenizing carbon colloid.Institute
Preparation method is stated to include the following steps:
By setting ratio, nitrogenous or sulfur-bearing hydrocarbons are added into nitridation carbon dust and mechanical mixture is uniform；
To the nitridation carbon dust and described nitrogenous or sulfur-bearing hydrocarbons progress ball milling after mixing, by setting
After fixed Ball-milling Time, uniform compound particles are formed；
By the method for ultrasonic agitation, the compound particles are dissolved；
Dialysis removes unreacted nitrogenous or sulfur-bearing hydrocarbons in the compound particles, obtains the nitridation carbon paste
Body.
Optionally, the method also includes: according to it is described nitridation carbon colloid concentration and dispersion effect determine the setting
Ratio.
Optionally, the weight ratio of the nitridation carbon dust and described nitrogenous or sulfur-bearing the hydrocarbons of addition is 1:10
To 1:100.
Optionally, the nitridation carbon dust is reacted the bulk of setting time acquisition by carbon nitrogen source presoma at a set temperature
Carbonitride grinds to be formed.
Optionally, the set temperature is 500 to 650 degrees Celsius, and the setting time is 1-10 hours.
Optionally, the carbon nitrogen source presoma and described nitrogenous or sulfur-bearing hydrocarbons are selected from urea, thiocarbamide, trimerization
One of cyanamide, cyanamide, guanidine hydrochloride and dicyandiamide are a variety of.
Optionally, the dialysis removes unreacted nitrogenous or sulfur-bearing hydrocarbons in the compound particles, specifically
Include:
It takes the dissolved upper turbid solution of the compound particles and is placed in bag filter；
The bag filter is placed in dialysis solvent and is dialysed, after the dialysis time of setting, obtains the nitridation
Carbon colloid.
Optionally, the aperture of the bag filter is 3500kDa；The dialysis time is 1-15 days；The dialysis solvent is
Water, ethyl alcohol or methanol.
Optionally, the revolving speed of the ball milling is 500-1000rpm；The Ball-milling Time is 5-30 hours.
Carbonitride colloid preparation method provided in an embodiment of the present invention makes colloid surface have hydrophilic functional groups abundant.
The preparation method has the advantages that yield is high, concentration is big, is convenient for regulation and simple process, and it is raw to can be applied to large-scale industry
It produces.
Finally preparing nitridation carbon colloid can be applied to various indoor hardware fittings or is carried on other catalyst loads
On body and in Material Manufacturing Process, the carbonitride colloidal materials are added as effective auxiliary agent, carbonitride is made
It is applied to many different fields such as indoor air purification for visible-light photocatalysis material, is with a wide range of applications, applies
Environmental protection and antimicrobial product in the fields such as chemical industry, daily use chemicals, medical, agriculture can be specifically used for air cleaning, sewage treatment, water body
The chemical fields such as antibacterial, the cosmetic product such as moisturizing cosmetic, moisture saver mask, suncream, the medical life such as medical antibacterial, Wound protection
Object material, the agricultural application such as soil remediation, water and soil moisturizer, soilless cultivation, plant growth, gel material is by ep-type material
Preparation, can be avoided the harm for environment, and play Environmental Role.
Detailed description of the invention
One or more embodiments are illustrated by the picture in corresponding attached drawing, these exemplary theorys
The bright restriction not constituted to embodiment, the element in attached drawing with same reference numbers label are expressed as similar element.It removes
Non- to have special statement, composition does not limit the figure in attached drawing.
Fig. 1 is the method flow diagram of the preparation method of the nitridation carbon colloid of the specific embodiment of the invention.
Specific embodiment
To make the purpose of the present invention, technical solution and effect clearer, clear and definite, right as follows in conjunction with drawings and embodiments
The present invention is further described.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to
Limit the present invention.
The numerical value disclosed in the embodiment of the present invention is approximation, and and non-determined value.Allow in error or experiment condition
In the case where, it may include all values in error range and be not limited to specific value disclosed in the embodiment of the present invention.
The numberical range disclosed in the embodiment of the present invention is for indicating the relative quantity of component in the mixture and its other party
The range of the temperature or other parameters enumerated in method embodiment.One or more numerical point in the numberical range is appropriate
Under conditions of obtain.
Nitridation carbon colloid refers to that carbonitride is dispersed in and formed in the solvent of suitable type, the stabilization with Tyndall effect
System.It plays important function served as bridge in the application of visible-light photocatalysis material in carbonitride.Fig. 1 is that the present invention is implemented
The method flow diagram of the preparation method for the nitridation carbon colloid that example provides.The preparation method is high with yield, concentration is big and technique is simple
Single feature.
As shown in Figure 1, the preparation method may include steps of:
110, setting ratio is pressed, nitrogenous or sulfur-bearing hydrocarbons is added into nitridation carbon dust and mechanical mixture is uniform.
Nitrogenous or sulfur-bearing the hydrocarbons can be it is any suitable, for providing the compound of nitrogen or sulphur functional group.
These nitrogen or sulphur functional group can modify on the surface of nitridation carbon dust and be stablized with helping preferably to be formed after reaction
Colloid.
Setting ratio is an empirical numerical value, can be it is any suitable, for indicating nitridation carbon dust and nitrogenous
Or between the hydrocarbons of sulfur-bearing ratio parameter, such as nitridation carbon dust and nitrogenous or sulfur-bearing hydrocarbons weight ratio
Example.Specifically, technical staff can determine the setting ratio according to the concentration of the nitridation carbon colloid and dispersion effect.
The setting ratio is a technological parameter, can by technical staff according to the needs of actual conditions, by experiment and/
Or the mode of reckoning etc. is configured.Preferably, described nitrogenous or sulfur-bearing the hydrocarbons of the nitridation carbon dust and addition
Weight ratio be 1:10 to 1:100 to prepare the nitridation carbon colloid that can satisfy concentration and dispersion effect requirement.
In some embodiments, when the nitridation carbon dust can be reacted setting at a set temperature by carbon nitrogen source presoma
Between the blocky carbonitride that obtains grind to be formed.
Grinding is the technical process for using mechanical system that blocky carbonitride is crushed to the nitridation carbon particle for suitable dimension,
It can specifically be realized using various ways.
Specific set temperature and setting time are the technological parameters according to circumstances debugged and set.Preferably, can
To select the set temperature as 500 to 650 degrees Celsius, the setting time control is between 1-10 hours, to obtain
Size or granularity suitably nitrogenize carbon dust.
In some embodiments, the carbon nitrogen source presoma and described nitrogenous or sulfur-bearing hydrocarbons can be selected from urine
One of element, thiocarbamide, melamine, cyanamide, guanidine hydrochloride and dicyandiamide are a variety of.It is preferred that technical staff can basis
Carbon nitrogen source presoma selects suitable nitrogenous or sulfur-bearing hydrocarbons to obtain preferably reaction and modification effect.
120, to the nitridation carbon dust and described nitrogenous or sulfur-bearing hydrocarbons progress ball milling after mixing, warp
After crossing the Ball-milling Time of setting, uniform compound particles are formed.
In mechanical milling process, nitridation carbon dust is easy to be generated exposed edges and defect abundant by mechanical damage, makes
The functional group for obtaining nitrogenous or sulfur-bearing hydrocarbons can very easily be grafted up.In addition, being produced during mechanical friction
Raw high temperature can also promote the grafting of surface functional group, so that nitridation carbon dust is modified by these functional groups.
The Ball-milling Time of a setting also empirical numerical value, can be by the need of technical staff according to the actual situation
It wants, is arranged by modes such as experimental verifications.It is preferred that amazing discovery, sets 500- for the revolving speed of ball milling
1000r.p.m, Ball-milling Time were controlled at 5-30 hours, can obtain preferable reaction effect, enabled nitridation carbon dust sufficient
It is reacted with nitrogenous or sulfur-bearing hydrocarbons.
130, by the method for ultrasonic agitation, the compound particles are dissolved.
The ultrasonic agitation can carry out in the solvent of any suitable type, such as water or other are suitable organic molten
Agent keeps compound particles fully dispersed in a solvent, achievees the effect that remove the impurity such as the presoma not reacted in mixture.
140, dialysis removes unreacted nitrogenous or sulfur-bearing hydrocarbons in the compound particles, obtains the nitridation
Carbon colloid.
Further unreacted nitrogenous or sulfur-bearing hydrocarbons are removed by the method for dialysis in step 140
To prepare pure nitridation carbon colloid.These nitridation carbon colloids are anti-by nitridation carbon dust and nitrogenous or sulfur-bearing hydrocarbons
It should obtain, surface graft has the functional group of modification, has extraordinary dispersibility.
In some embodiments, the method for the dialysis can be specifically achieved by the steps of:
Firstly, taking the dissolved upper turbid solution of the compound particles.
The impurity such as the presoma not reacted due to dispersibility etc. problem, and insoluble in solvent.Therefore, muddy in absorption
After turbid, the first separation for compound particles can be realized.
Then, turbid solution on this is placed in bag filter to be placed in dialysis solvent and is dialysed.
Bag filter is can to function similarly to the effect of sieve selectively penetrating pocket made of film.It is molten dialysing
Under the osmotic pressure effect of liquid, unreacted nitrogenous or sulfur-bearing hydrocarbons are precipitate into dialysis solvent in turbid solution in order.
Specifically, the aperture of the bag filter can be 3500kDa.The dialysis solvent is water, ethyl alcohol or methanol.When
So, technical staff can also select suitable bag filter according to the molecular dimension of nitrogenous or sulfur-bearing the hydrocarbons of actual use
Aperture.
Finally, obtaining the nitridation carbon colloid after the dialysis time of setting.It is stagnant after sufficient dialysis time
The liquid stayed in bag filter is pure nitridation carbon colloid, and unreacted nitrogenous or sulfur-bearing hydrocarbons can be gone
It removes.
Specifically, the dialysis time is 1-15 days, so that unreacted nitrogenous or sulfur-bearing hydrocarbons are abundant
Removal.
Carbonitride colloid preparation method provided in an embodiment of the present invention makes colloid surface have hydrophilic functional groups abundant.
Entire preparation has the advantages that yield is high, concentration is big, is convenient for regulation and simple process, can be applied to large-scale industrial production.
It should be noted that the preparation of extensive colloid equally may be implemented using the preparation method of other colloids, such as
The chemical methodes such as acidization, alkalization method, coacervation, the precipitation method；The physics sides such as ball-milling method, ultrasonic dispersion, polymer dispersion method
Method.
The embodiment of the present invention finally prepare nitridation carbon colloid be with a wide range of applications, be applied to chemical industry, daily use chemicals,
The environmental protection in the fields such as medical, agriculture and antimicrobial product can be specifically used for the chemical industry such as air cleaning, sewage treatment, water body antibacterial neck
Domain, the cosmetic product such as moisturizing cosmetic, moisture saver mask, suncream, the biomaterial for medical purpose such as medical antibacterial, Wound protection, soil
The agricultural application such as reparation, water and soil moisturizer, soilless cultivation, plant growth, gel material are prepared by ep-type material, can be kept away
Exempt from the harm for environment, and plays Environmental Role.
Preparation method based on the embodiment of the present invention provides the preparating example of multiple nitridation carbon colloids, sufficiently to say
The preparation process of bright nitridation carbon colloid.
Embodiment 1:
1) crucible is added as carbon nitride precursor in melamine and be placed in Muffle furnace, forged under the conditions of 550 DEG C
Burn 2h.
2) it after waiting melamine to be cooled to room temperature, takes out and using mortar grinder 1.5h from Muffle furnace to be nitrogenized
Carbon dust.
3) 5.0g nitridation carbon dust and 300g urea are put into after evenly mixing in ball mill, with the condition of 700r.p.m,
Ball milling 10h is to obtain compound particles.
4) by ultrasonic agitation dissolution, the compound particles are dispersed in 500ml water.
5) the dissolved upper suspension of ultrasonic agitation is taken, and puts it into the bag filter that aperture is 3500KDa and carries out
Dialysis.
6) it after dialysis after a week, takes out the suspension in bag filter and demarcates carbonitride colloid concentration.
7) the water body purification performance for nitrogenizing carbon colloid, applied to the environmental protection in the fields such as chemical industry, daily use chemicals, medical, agriculture and anti-
Bacterium product, can be specifically used for the chemical fields such as air cleaning, sewage treatment, water body antibacterial, and moisturizing cosmetic, is prevented moisture saver mask
Shine the cosmetic product such as frost, the biomaterial for medical purpose such as medical antibacterial, Wound protection, soil remediation, water and soil moisturizer, soilless cultivation,
The agricultural application such as plant growth.
Embodiment 2:
1) crucible is added as carbon nitride precursor in dicyandiamide and be placed in Muffle furnace, calcined under the conditions of 600 DEG C
2h。
2) it after waiting dicyandiamide to be cooled to room temperature, takes out and using mortar grinder 1.5h from Muffle furnace to obtain carbonitride
Powder.
3) 10.0g nitridation carbon dust and 300g thiocarbamide are put into after evenly mixing in ball mill, with the item of 1000r.p.m
Part, ball milling 20h is to obtain compound particles.
4) by ultrasonic agitation dissolution, the compound particles are dispersed in 1000ml water.
5) the dissolved upper suspension of ultrasonic agitation is taken, and puts it into the bag filter that aperture is 3500KDa and carries out
Dialysis.
6) it after dialysis after a week, takes out the suspension in bag filter and demarcates carbonitride colloid concentration.
7) antibacterial characteristics of colloid are excellent, environmental protection and antimicrobial product applied to the fields such as chemical industry, daily use chemicals, medical, agriculture,
It can be specifically used for the chemical fields such as air cleaning, sewage treatment, water body antibacterial, moisturizing cosmetic, moisture saver mask, suncream etc. are changed
Cosmetics, the biomaterial for medical purpose such as medical antibacterial, Wound protection, soil remediation, water and soil moisturizer, soilless cultivation, plant growth
It is applied Deng agricultural.
Embodiment 3:
1) crucible is added as carbon nitride precursor in urea and be placed in Muffle furnace, calcine 2h under the conditions of 500 DEG C.
2) it after waiting urea to be cooled to room temperature, takes out and using mortar grinder 1.5h from Muffle furnace to obtain nitridation carbon dust
End.
3) 5.0g nitridation carbon dust and 300g urea are put into after evenly mixing in ball mill, with the condition of 500r.p.m,
Ball milling 20h is to obtain compound particles.
4) by ultrasonic agitation dissolution, the compound particles are dispersed in 500ml ethyl alcohol.
5) the dissolved upper suspension of ultrasonic agitation is taken, and puts it into the bag filter that aperture is 3500KDa and carries out
Dialysis.
6) it after dialysis after a week, takes out the suspension in bag filter and demarcates carbonitride colloid concentration.
7) gel prepared has high antibiotic property, environmental protection and antibacterial applied to the fields such as chemical industry, daily use chemicals, medical, agriculture
Product, can be specifically used for the chemical fields such as air cleaning, sewage treatment, water body antibacterial, moisturizing cosmetic, moisture saver mask, sun-proof
The cosmetic product such as frost, the biomaterial for medical purpose such as medical antibacterial, Wound protection, soil remediation, water and soil moisturizer, soilless cultivation, plant
The agricultural application such as object growth.
Embodiment 4:
1) it takes 15g melamine as carbon nitride precursor, crucible is added and is placed in Muffle furnace, in 400 DEG C of conditions
Lower calcining 2.5h.
2) it after waiting melamine to be cooled to room temperature, takes out and using mortar grinder 1h from Muffle furnace to obtain carbonitride
Powder.
3) 5.0g nitridation carbon dust and 300g urea are put into after evenly mixing in ball mill, with the condition of 500r.p.m,
Ball milling 2h is to obtain compound particles.
4) by ultrasonic agitation dissolution, the compound particles are dispersed in 500ml ethyl alcohol.
5) the dissolved upper suspension of ultrasonic agitation is taken, and puts it into the bag filter that aperture is 3500KDa and carries out
Dialysis.
6) it after dialysis after a week, takes out the suspension in bag filter and demarcates carbonitride colloid concentration.
7) it takes 6.908g nickel foam and impregnates 2h in concentrated acid.
8) after concentrated acid immersion, successively nickel foam is impregnated 3 times in ultrapure water, organic solution is impregnated 1 time.
9) it dries the nickel foam and is soaked in the nitridation carbon colloid prepared.
10) using drying station under 40 DEG C of constant temperature, drying is soaked in the nickel foam in the nitridation carbon colloid.
11) it is repeated several times after step 9 and step 10, prepares monoblock type catalysis material.
12) air cleaning of the monoblock type catalysis material obtained, water body purification and anti-microbial property are excellent, are suitable for refrigerator
Deodorization, shoe chest antibacterial and deodouring, lavatory such as eliminate the unusual smell at the domestic environments, such as deodorant for refregerator packet, the agent of shoe chest antibacterial purifying, toilet remove
Peculiar smell box etc..
Embodiment 5:
1) crucible is added as carbon nitride precursor in urea and be placed in Muffle furnace, calcine 2h under the conditions of 500 DEG C.
2) it after waiting urea to be cooled to room temperature, takes out and using mortar grinder 1.5h from Muffle furnace to obtain nitridation carbon dust
End.
3) 10.0g nitridation carbon dust and 300g urea are put into after evenly mixing in ball mill, with the item of 500r.p.m
Part, ball milling 20h is to obtain compound particles.
4) by ultrasonic agitation dissolution, the compound particles are dispersed in 500ml ethyl alcohol,.
5) the dissolved upper suspension of ultrasonic agitation is taken, and puts it into the bag filter that aperture is 3500KDa and carries out
Dialysis.
6) it after dialysis after a week, takes out the suspension in bag filter and demarcates carbonitride colloid concentration.
7) the nitridation carbon colloid in bag filter is put into aging 36h in 60 DEG C of thermostat water bath, obtains carbonitride water-setting
Glue.
8) the carbonitride hydrogel obtained is applied to environmental protection and the antimicrobial product in the fields such as chemical industry, daily use chemicals, medical, agriculture,
It can be specifically used for the chemical fields such as air cleaning, sewage treatment, water body antibacterial, moisturizing cosmetic, moisture saver mask, suncream etc. are changed
Cosmetics, the biomaterial for medical purpose such as medical antibacterial, Wound protection, soil remediation, water and soil moisturizer, soilless cultivation, plant growth
It is applied Deng agricultural.
Embodiment 6:
1) crucible is added as carbon nitride precursor in urea and be placed in Muffle furnace, calcine 3h under the conditions of 550 DEG C.
2) after being cooled to room temperature, 10.0g nitridation carbon dust and 300g urea are put into ball mill after evenly mixing, with
The condition of 500r.p.m, liquid phase ball milling 20h is to obtain nitridation carbon solution.
3) the dissolved upper suspension of ultrasonic agitation is taken, and puts it into the bag filter that aperture is 3500KDa and carries out
Dialysis.
4) dialyse a Zhou Yihou, takes out the suspension in bag filter and demarcates carbonitride colloid concentration.
5) the nitridation carbon colloid in bag filter is put into aging in 60 DEG C of thermostat water bath and for 24 hours, obtains carbonitride gel.
6) emulsion form, paste is presented in the carbonitride gel obtained, for the excellent of Escherichia coli, staphylococcus aureus etc.
Antibacterial characteristics, environmental protection and antimicrobial product applied to the fields such as chemical industry, daily use chemicals, medical, agriculture, can be specifically used for air cleaning,
The chemical fields such as sewage treatment, water body antibacterial, the cosmetic product such as moisturizing cosmetic, moisture saver mask, suncream, medical antibacterial, wound
The biomaterial for medical purpose such as mouth protection, the agricultural application such as soil remediation, water and soil moisturizer, soilless cultivation, plant growth.
Embodiment 7:
1) under conditions of magnetic agitation, 5mL copper-bath (concentration 0.2mol/L) is rapidly joined into 10.0g nitridation
In carbon dust and 300g urea mixed solution, with the condition of 500r.p.m, liquid phase ball milling 20h is to obtain solution.
2) the dissolved upper suspension of ultrasonic agitation is taken, and puts it into the bag filter that aperture is 3500KDa and carries out
Dialysis.
3) dialyse a Zhou Yihou, takes out the suspension in bag filter and demarcates carbonitride colloid concentration.
4) the nitridation carbon colloid in bag filter is put into aging in 60 DEG C of thermostat water bath and for 24 hours, obtains carbonitride gel.
5) hydrogel material is put into freeze drier and is freeze-dried, obtain aerogel material.
6) it step 5) is prepared into aerogel material is put into ptfe autoclave and seal, be placed at 160 DEG C
Heating 4 hours.
7) after being cooled to room temperature, the aerogel material of the pre-heat treatment is taken out, in argon atmosphere, 550 DEG C of calcinings 4 are small
When, obtain CuO@g-C3N4Photocatalysis aerogel material.
8) to CuO@g-C3N4Photocatalysis aerogel material carries out photocatalysis antibacterial active testing:
Firstly, by CuO@g-C3N4Photocatalysis aerogel material is pulverized last, and the sample sack of bacteria culture media is added
In.Then, the sample sack equipped with photocatalyzed gel material and bacteria culture media is placed under natural light, at interval of the scheduled time
Bacteria culture media is observed and recorded.
The photocatalysis aeroge of preparation has the anti-microbial properties such as excellent Escherichia coli, staphylococcus aureus, has wide
It is net can be specifically used for air for the potentiality of general application, environmental protection and antimicrobial product applied to the fields such as chemical industry, daily use chemicals, medical, agriculture
The chemical fields such as change, sewage treatment, water body antibacterial, the cosmetic product such as moisturizing cosmetic, moisture saver mask, suncream, medical antibacterial,
The biomaterial for medical purpose such as Wound protection, the agricultural application such as soil remediation, water and soil moisturizer, soilless cultivation, plant growth, gelinite
Material is prepared by ep-type material, can be avoided the harm for environment, and play Environmental Role.
The concentration range of the nitridation carbon colloid prepared in above-described embodiment 1-7 in water is 0.5mg/ml-30mg/
Ml has good dispersibility.And surface has hydrophilic functional groups abundant, it can be made to have with other materials good
Associativity.
Although the embodiment of the present invention only for preparing carbonitride hydrogel and monoblock type catalysis material, describes the nitrogen
Change the application of carbon colloid.It will be appreciated by those skilled in the art that the nitridation carbon colloid can also be passed through other
Different preparation processes, the purposes different applied to other or prepares different types of material.
It, can according to the technique and scheme of the present invention and this hair it is understood that for those of ordinary skills
Bright design is subject to equivalent substitution or change, and all these changes or replacement all should belong to the guarantor of appended claims of the invention
Protect range.
Claims (10)
1. a kind of preparation method for nitrogenizing carbon colloid characterized by comprising
By setting ratio, nitrogenous or sulfur-bearing hydrocarbons are added into nitridation carbon dust and mechanical mixture is uniform；
To the nitridation carbon dust and described nitrogenous or sulfur-bearing hydrocarbons progress ball milling after mixing, by setting
After Ball-milling Time, uniform compound particles are formed；
By the method for ultrasonic agitation, the compound particles are dissolved；
Dialysis removes unreacted nitrogenous or sulfur-bearing hydrocarbons in the compound particles, obtains the nitridation carbon colloid.
2. preparation method according to claim 1, which is characterized in that the method also includes: according to the nitridation carbon paste
The concentration and dispersion effect of body determine the setting ratio.
3. preparation method according to claim 2, which is characterized in that the nitridation carbon dust and addition described nitrogenous or
The weight ratio of the hydrocarbons of sulfur-bearing is 1:10 to 1:100.
4. preparation method according to claim 1, which is characterized in that the nitridation carbon dust is being set by carbon nitrogen source presoma
The blocky carbonitride for determining to react setting time acquisition at temperature grinds to be formed.
5. the preparation method according to claim 4, which is characterized in that the set temperature is 500 to 650 degrees Celsius, institute
Stating setting time is 1-10 hours.
6. the preparation method according to claim 4, which is characterized in that the method also includes: according to the nitridation carbon dust
The carbon nitrogen source presoma at end determines described nitrogenous or sulfur-bearing hydrocarbon.
7. the preparation method according to claim 4, which is characterized in that the carbon nitrogen source presoma and described nitrogenous or sulfur-bearing
Hydrocarbons be selected from one of urea, thiocarbamide, melamine, cyanamide, guanidine hydrochloride and dicyandiamide or a variety of.
8. preparation method according to claim 1, which is characterized in that the dialysis removes not anti-in the compound particles
Nitrogenous or sulfur-bearing the hydrocarbons answered, specifically include:
It takes the dissolved upper turbid solution of the compound particles and is placed in bag filter；
The bag filter is placed in dialysis solvent and is dialysed, after the dialysis time of setting, obtains the nitridation carbon paste
Body.
9. preparation method according to claim 8, which is characterized in that the aperture of the bag filter is 3500kDa；It is described
Analysing the time is 1-15 days；The dialysis solvent is water, ethyl alcohol or methanol.
10. preparation method according to claim 1, which is characterized in that the revolving speed of the ball milling is 500-1000r.p.m；
The Ball-milling Time is 5-30 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910138693.3A CN109847785A (en) | 2019-02-25 | 2019-02-25 | A kind of preparation method nitrogenizing carbon colloid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910138693.3A CN109847785A (en) | 2019-02-25 | 2019-02-25 | A kind of preparation method nitrogenizing carbon colloid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109847785A true CN109847785A (en) | 2019-06-07 |
Family
ID=66898940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910138693.3A Pending CN109847785A (en) | 2019-02-25 | 2019-02-25 | A kind of preparation method nitrogenizing carbon colloid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109847785A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111573636A (en) * | 2020-05-19 | 2020-08-25 | 江南大学 | Application of carbon nitride material as plant fertilizer in promoting photosynthesis |
| CN111795875A (en) * | 2019-04-08 | 2020-10-20 | 南京工业大学 | Preparation method of soil colloid particles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104401948A (en) * | 2014-11-17 | 2015-03-11 | 长安大学 | Preparation method for single-layer graphite-type carbon nitride nanosheet solution |
| CN107486231A (en) * | 2017-08-24 | 2017-12-19 | 福州大学 | A kind of preparation method of graphite phase carbon nitride colloid photochemical catalyst |
-
2019
- 2019-02-25 CN CN201910138693.3A patent/CN109847785A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104401948A (en) * | 2014-11-17 | 2015-03-11 | 长安大学 | Preparation method for single-layer graphite-type carbon nitride nanosheet solution |
| CN107486231A (en) * | 2017-08-24 | 2017-12-19 | 福州大学 | A kind of preparation method of graphite phase carbon nitride colloid photochemical catalyst |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111795875A (en) * | 2019-04-08 | 2020-10-20 | 南京工业大学 | Preparation method of soil colloid particles |
| CN111573636A (en) * | 2020-05-19 | 2020-08-25 | 江南大学 | Application of carbon nitride material as plant fertilizer in promoting photosynthesis |
| CN111573636B (en) * | 2020-05-19 | 2021-11-02 | 江南大学 | Application of carbon nitride material as plant fertilizer in promoting photosynthesis |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104841015B (en) | High-specific-surface-area silver-loaded titanium dioxide composite antibacterial material and preparation method thereof | |
| CN104588061B (en) | Preparation method based on the photocatalyst of titanium dioxide activated carbon that g-carbonitride is combined | |
| CN109847785A (en) | A kind of preparation method nitrogenizing carbon colloid | |
| CN104069879A (en) | Preparation method for titanium dioxide/hydroxyapatite composite photocatalyst | |
| CN105295105A (en) | Bacterial cellulose based composite material having photocatalytic antibacterial property | |
| CN107983353B (en) | TiO 22-Fe2O3Preparation method and application of composite powder | |
| CN107522169A (en) | A kind of normal temperature prepares pure organic homogeneous precipitation method of nano-oxide | |
| CN104927097B (en) | A kind of method that microwave-hydrothermal method prepares nano titanium oxide/Chitosan Composites | |
| CN108187466A (en) | A kind of advanced oxidation coupled biological cleaning system and its application based on ozone regulation and control | |
| CN107262051B (en) | Carboxymethyl Konjac Glucomannan microsphere adsorbing agent and preparation method thereof for dephosphorization | |
| CN111744503A (en) | Z-shaped heterojunction MoS2/Bi2WO6Composite photocatalyst and preparation method and application thereof | |
| CN109622020A (en) | A kind of photocatalyzed gel material and preparation method thereof | |
| CN103539121B (en) | Porous carbonate and porous oxide preparation methods | |
| Xu et al. | Study on visible light photocatalytic performance of BiVO4 modified by graphene analogue boron nitride | |
| CN106189146A (en) | A kind of preparation method of polylactic acid antibacterial matrices | |
| CN106186368A (en) | A kind of preparation method of saprobia fermentation process agent | |
| CN110938230B (en) | Multifunctional foamed natural rubber with high catalytic performance and antibacterial performance and preparation method thereof | |
| Bao et al. | Synthesis and antibacterial activities of Ag-TiO2/ZIF-8 | |
| DE50003904D1 (en) | MOLDED BODIES OF TITANIUM DIOXIDE, METHOD FOR THE PRODUCTION AND USE THEREOF | |
| CN107199046B (en) | A kind of preparation method of three four/titanium dioxide composite photocatalyst of nitrogen of g- carbon of sandwiched configuration | |
| CN101676030B (en) | Method for preparing photocatalyst with core-shell structure | |
| CN109354915A (en) | The environmental protection type nano material multifunctional water and preparation method thereof of the water-soluble finishing product of dilution | |
| CN110028364A (en) | A kind of efficient soil conditioning granule and its preparation method and application | |
| CN108654664A (en) | A kind of emulation plant and preparation method with visible light-responded catalysis | |
| CN105236532B (en) | The preparation method of microcrystalline cellulose/γ polyglutamic acid nano silver composite materials |
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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200722 Address after: No.8-122002, Xindu Avenue, Xindu District, Chengdu, Sichuan 610500 Applicant after: Zhao Ziyan Applicant after: Wan Wenchao Applicant after: Zhao Ziquan Address before: 643200 No. 33-4 Guihua Street, Fushun County, Zigong City, Sichuan Province Applicant before: Mou Fushu |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190607 |