CN107651659A - The preparation method of antibiotic property hydroxyl cupric phosphate - Google Patents
The preparation method of antibiotic property hydroxyl cupric phosphate Download PDFInfo
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- CN107651659A CN107651659A CN201710958238.9A CN201710958238A CN107651659A CN 107651659 A CN107651659 A CN 107651659A CN 201710958238 A CN201710958238 A CN 201710958238A CN 107651659 A CN107651659 A CN 107651659A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of preparation method of antibiotic property hydroxyl cupric phosphate, comprise the following steps:Step 1: pressing parts by volume, the inorganic copper salt solution that 20~30 parts of mass fractions are 40~60% is added in the acid-phosphate solution that 40~60 parts of mass fractions are 40~60%, stirs 30~60min;Then NH is added3·H2O adjusts pH to 2.5~7;Step 2: the solution after regulation pH is transferred into stainless steel cauldron, reacted 1~3 hour at 165~185 DEG C, cool down, be then centrifuged for, obtained solid is cleaned with deionized water, is dried, is obtained antibiotic property hydroxyl cupric phosphate.The preparation method of the present invention has the characteristics that synthetic method is simple and convenient to operate, raw material is environmentally friendly, yield is high, easily scattered, and beneficial to large-scale industrial production is realized, the hydroxyl cupric phosphate of synthesis has excellent anti-microbial property.
Description
Technical field
The present invention relates to a kind of preparation method of hydroxyl cupric phosphate, and in particular to a kind of preparation of antibiotic property hydroxyl cupric phosphate
Method.
Background technology
Hydroxyl cupric phosphate is the new catalytic material of a kind of low surface area, pore-free and hollow structure, in oxidation of alcohols, phenol
Hydroxylation, epoxidation of styrene, cyclohexane oxidation, catalysis H2O2Processing sewage and photocatalysis etc. show good catalytic
Can, it also has, and cost is low, catalytic activity is high, mild condition, product are easily separated and the advantages such as catalytic process is clean, has wide
Application prospect.At present, the preparation of hydroxyl cupric phosphate mainly uses hydro-thermal method, using copper acetate, phosphoric acid and ethylenediamine as raw material, water
Thermal crystallisation 3d is obtained.This method uses excess phosphoric acid, and the excessive emissions of phosphorus make aqueous systems eutrophication, destroy water ecology and follow
Ring balances, and causes water quality deterioration;In addition, ethylenediamine is volatile organic amine, to the toxic effect of human body.
Natural di copper mineral is referred to as liebethenite, degrading organic dye waste water and phenol hydroxyl in a mild condition
Excellent catalytic performance is shown during base.Compared with other heterogeneous catalysis, hydroxyl cupric phosphate, which has, prepares cost
It is low, catalytic activity is higher, is easy to the advantages such as product separation, catalytic process more cleaning, there is broader practice prospect.
Hydroxyl cupric phosphate is a kind of new catalytic material with applications well prospect, is applied to methylene under visible ray
The blue degraded of base, its performance are superior to commodity micron/nanometer titanium dioxide P25 and tungsten oxide.Relevant copper hydroxyphosphate catalyst powder
Preparation method require higher, it is necessary to add conditioning agent for raw material and reaction condition, operate more complicated, obtained catalyst
Powder catalytic effect is not ideal enough or catalytic cycle is grown, or even the method having has the wave that raw material is easily caused in preparation process
The shortcomings of taking and polluting.
At present, had not been reported for research of the hydroxyl cupric phosphate as antiseptic, the present invention passes through the simply side of synthesis
Method, it is prepared for a kind of antibiotic property hydroxyl cupric phosphate.
The content of the invention
It is an object of the invention to solve at least the above and/or defect, and provide at least will be described later it is excellent
Point.
In order to realize according to object of the present invention and further advantage, there is provided a kind of system of antibiotic property hydroxyl cupric phosphate
Preparation Method, comprise the following steps:
Step 1: pressing parts by volume, the inorganic copper salt solution that 20~30 parts of mass fractions are 40~60% is added 40~60
Part mass fraction is in 40~60% acid-phosphate solution, stirs 30~60min;Then NH is added3·H2O adjust pH to
2.5~7;
Step 2: the solution after regulation pH is transferred into stainless steel cauldron, reacted 1~3 hour at 165~185 DEG C,
Cooling, is then centrifuged for, and obtained solid is cleaned with deionized water, is dried, is obtained antibiotic property hydroxyl cupric phosphate.
Preferably, the inorganic copper salt solution is any one in copper nitrate solution, copper chloride solution, copper-bath
Kind.
Preferably, the acid-phosphate solution be ammonium hydrogen phosphate solution, dibastic sodium phosphate solution, phosphoric acid hydrogen potassium solution,
Any one in sodium dihydrogen phosphate, potassium dihydrogen phosphate.
Preferably, the rotating speed used that centrifuges is 5000rpm, time 15min.
Preferably, the process of the step 1 replaces with:By the Inorganic Copper that 20~30 parts of mass fractions are 40~60%
Salting liquid is injected into the spray containers I with stainless steel shower nozzle and is fixed on the propulsion pump I for being provided with high voltage electrostatic equipment;Together
When by 20~30 parts of mass fractions be 40~60% acid-phosphate solution be injected into the spray containers II with stainless steel shower nozzle
In and be fixed on the propulsion pump II for being provided with high voltage electrostatic equipment;By weight, 1~5 part of surfactant is dissolved in 20
The acid-phosphate solution that~30 parts of mass fractions are 40~60%, is then inserted in the reactor with agitating device;Spraying
High pressure is set using high voltage electrostatic equipment on the stainless steel syringe needle of container I and spray containers II, while is set and is promoted pump I and promote
The fltting speed of pump II, inorganic copper salt solution and acid-phosphate solution are instilled in reactor with drop state simultaneously;In liquid
While drop instills reactor, stirring reaction, after drop is added dropwise to complete, continue 10~30min of stirring, to anti-while stirring
Answer and ammonia is passed through in device, adjust pH to 2.5~7.
Preferably, the internal diameter of described stainless steel shower nozzle is 0.5~1.2mm;Described promotes pump I and propulsion pump II
Fltting speed is 15~20mL/h;High pressure size is 3-8kV.
Preferably, the surfactant includes the raw material of following parts by weight:5~10 parts of polyvinylpyrrolidones, 0.5
~1 part of nonyl phenol, 0.3~0.5 part of 1- ethyl-3-methylimidazoles lactic acid, 1~3 part of alkyl dimethyl betaine, 0.2~0.5 part
APG, 1~3 part of dodecyl benzyl dimethyl ammonium chloride.
Preferably, in the step 2, before cooling, reaction solution is added in stainless steel spherical container, will be spherical
Container is placed on four axle bevellers, opens four axle bevellers, drives stainless steel spherical container randomly to rotate, and reacts 30~60min;
The charging aperture of the stainless steel spherical container is sealed by threaded cap, the table after threaded cap sealed connection with stainless steel spherical container
Face flushes;The active rotating speed of the four axles beveller is 100~150rpm, and stochastic transition frequency is 10~30s.
Preferably, the drying is dried using microwave radiation, and its process is:It is dry that reactant after cleaning is put into quartz
In dry device, it is subsequently placed in microwave radiation reacting furnace;Nitrogen is passed through with 50~100mL/min speed, microwave is carried out to precipitation
Radiant drying processing;The condition of the microwave radiation drying process is:Microwave radiation frequencies are 2450 ± 50MHz, microwave radiation
Unit power is 0.10~1.00w/g, and microwave irradiation time is 30~60min, and microwave radiation temperature is 50~70 DEG C.
The present invention also provides a kind of antibiotic property hydroxyl cupric phosphate that above-mentioned preparation method obtains in Escherichia coli are killed
Application.
The present invention comprises at least following beneficial effect:The present invention preparation method there is synthetic method to be simple and convenient to operate,
The features such as raw material environmental protection, high, easily scattered yield, beneficial to realizing large-scale industrial production, the hydroxyl cupric phosphate of synthesis has excellent
Different anti-microbial property.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings:
Fig. 1 is the SEM figures of hydroxyl cupric phosphate prepared by the embodiment of the present invention 1;
Fig. 2 is the EDX figures of hydroxyl cupric phosphate prepared by the embodiment of the present invention 1;
Fig. 3 is the SEM figures of hydroxyl cupric phosphate prepared by the embodiment of the present invention 2;
Fig. 4 is the SEM figures of hydroxyl cupric phosphate prepared by the embodiment of the present invention 3.
Embodiment:
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of individual other elements or its combination.
Embodiment 1:
A kind of preparation method of antibiotic property hydroxyl cupric phosphate, comprises the following steps:
Step 1: pressing parts by volume, the copper nitrate solution that 25 parts of mass fractions are 50% is added into 50 parts of mass fractions is
In 50% dibastic sodium phosphate solution, 30min is stirred;Then NH is added3·H2O adjusts pH to 2.5;
Step 2: the solution after regulation pH is transferred into stainless steel cauldron, react 2 hours, cool down, so at 180 DEG C
After centrifuge, obtained solid is cleaned with deionized water, dry, obtain antibiotic property hydroxyl cupric phosphate;The rotating speed that the centrifugation uses
For 5000rpm, time 15min.
Embodiment 2:
A kind of preparation method of antibiotic property hydroxyl cupric phosphate, comprises the following steps:
Step 1: pressing parts by volume, the copper nitrate solution that 25 parts of mass fractions are 50% is added into 50 parts of mass fractions is
In 50% dibastic sodium phosphate solution, 30min is stirred;Then NH is added3·H2O adjusts pH to 5;
Step 2: the solution after regulation pH is transferred into stainless steel cauldron, react 2 hours, cool down, so at 180 DEG C
After centrifuge, obtained solid is cleaned with deionized water, dry, obtain antibiotic property hydroxyl cupric phosphate;The rotating speed that the centrifugation uses
For 5000rpm, time 15min.
Embodiment 3:
A kind of preparation method of antibiotic property hydroxyl cupric phosphate, comprises the following steps:
Step 1: pressing parts by volume, the copper nitrate solution that 25 parts of mass fractions are 50% is added into 50 parts of mass fractions is
In 50% dibastic sodium phosphate solution, 30min is stirred;Then NH is added3·H2O adjusts pH to 7;
Step 2: the solution after regulation pH is transferred into stainless steel cauldron, react 2 hours, cool down, so at 180 DEG C
After centrifuge, obtained solid is cleaned with deionized water, dry, obtain antibiotic property hydroxyl cupric phosphate;The rotating speed that the centrifugation uses
For 5000rpm, time 15min.
Embodiment 4:
The process of the step 1 replaces with:By parts by volume, the copper nitrate solution that 25 parts of mass fractions are 50% is injected
Into the spray containers I with stainless steel shower nozzle and it is fixed on the propulsion pump I for being provided with high voltage electrostatic equipment;Simultaneously by 30 parts of matter
The dibastic sodium phosphate solution that amount fraction is 50%, which is injected into the spray containers II with stainless steel shower nozzle and is fixed on, is provided with high pressure
On the propulsion pump II of electrostatic apparatus;By weight, 3 parts of surfactants are dissolved in the phosphoric acid hydrogen that 20 parts of mass fractions are 50%
In sodium solution, then insert in the reactor with agitating device;It is sharp on the stainless steel syringe needle of spray containers I and spray containers II
High pressure is set with high voltage electrostatic equipment, while the fltting speed for promoting pump I and promoting pump II is set, by copper nitrate solution and phosphoric acid
Hydrogen sodium solution is instilled in reactor with drop state simultaneously;While drop instills reactor, stirring reaction, drop drips
Cheng Hou, continue to stir 30min, ammonia is passed through into reactor while stirring, adjusts pH to 5;Described stainless steel shower nozzle
Internal diameter be 0.5mm;Described propulsion pump I and the fltting speed of propulsion pump II are 15mL/h;High pressure size is 6kV.The table
Face activating agent includes the raw material of following parts by weight:5 parts of polyvinylpyrrolidones, 0.5 part of nonyl phenol, 0.3 part of 1- ethyl -3- methyl
Imidazole lactic acid, 1 part of alkyl dimethyl betaine, 0.2 part of APG, 1 part of dodecyl benzyl dimethyl ammonium chloride.Pass through electricity
Spray method and the surface activator composition added further change the crystalline structure of hydroxyl cupric phosphate, improve di
The antibiotic property of copper.
Remaining technological parameter and method with it is identical in embodiment 2.
Embodiment 5:
The process of the step 1 replaces with:By parts by volume, the copper nitrate solution that 25 parts of mass fractions are 50% is injected
Into the spray containers I with stainless steel shower nozzle and it is fixed on the propulsion pump I for being provided with high voltage electrostatic equipment;Simultaneously by 30 parts of matter
The dibastic sodium phosphate solution that amount fraction is 50%, which is injected into the spray containers II with stainless steel shower nozzle and is fixed on, is provided with high pressure
On the propulsion pump II of electrostatic apparatus;By weight, 5 parts of surfactants are dissolved in the phosphoric acid hydrogen that 20 parts of mass fractions are 50%
In sodium solution, then insert in the reactor with agitating device;It is sharp on the stainless steel syringe needle of spray containers I and spray containers II
High pressure is set with high voltage electrostatic equipment, while the fltting speed for promoting pump I and promoting pump II is set, by copper nitrate solution and phosphoric acid
Hydrogen sodium solution is instilled in reactor with drop state simultaneously;While drop instills reactor, stirring reaction, drop drips
Cheng Hou, continue to stir 10min, ammonia is passed through into reactor while stirring, adjusts pH to 5;Described stainless steel shower nozzle
Internal diameter be 0.5mm;Described propulsion pump I and the fltting speed of propulsion pump II are 20mL/h;High pressure size is 5kV.The table
Face activating agent includes the raw material of following parts by weight:10 parts of polyvinylpyrrolidones, 1 part of nonyl phenol, 0.5 part of 1- ethyl -3- methyl
Imidazole lactic acid, 3 parts of alkyl dimethyl betaines, 0.5 part of APG, 3 parts of dodecyl benzyl dimethyl ammonium chlorides.
Remaining technological parameter and method with it is identical in embodiment 2.
Embodiment 6:
In the step 2, before cooling, reaction solution is added in stainless steel spherical container, spherical container is placed in four
On axle beveller, four axle bevellers are opened, drive stainless steel spherical container randomly to rotate, react 30min;The stainless steel is spherical
The charging aperture of container is sealed by threaded cap, and threaded cap flushes after being tightly connected with the surface of stainless steel spherical container;Described four
The active rotating speed of axle beveller is 100rpm, and stochastic transition frequency is 10s.By in spherical container on four axle bevellers
Random rotation, the crystalline structure of hydroxyl cupric phosphate is changed, improve the antibiotic property of hydroxyl cupric phosphate.
Remaining technological parameter and method with it is identical in embodiment 2.
Embodiment 7:
In the step 2, before cooling, reaction solution is added in stainless steel spherical container, spherical container is placed in four
On axle beveller, four axle bevellers are opened, drive stainless steel spherical container randomly to rotate, react 60min;The stainless steel is spherical
The charging aperture of container is sealed by threaded cap, and threaded cap flushes after being tightly connected with the surface of stainless steel spherical container;Described four
The active rotating speed of axle beveller is 150rpm, and stochastic transition frequency is 30s.
Remaining technological parameter and method with it is identical in embodiment 2.
Embodiment 8:
The drying is dried using microwave radiation, and its process is:Reactant after cleaning is put into quartzy drier, so
After be placed in microwave radiation reacting furnace;Nitrogen is passed through with 100mL/min speed, microwave radiation drying process is carried out to precipitation;
The condition of the microwave radiation drying process is:Microwave radiation frequencies are 2450 ± 50MHz, and microwave radiation unit power is
1.00w/g, microwave irradiation time 30min, microwave radiation temperature are 50 DEG C.
Remaining technological parameter and method with it is identical in embodiment 2.
Embodiment 9:
The drying is dried using microwave radiation, and its process is:Reactant after cleaning is put into quartzy drier, so
After be placed in microwave radiation reacting furnace;Nitrogen is passed through with 50mL/min speed, microwave radiation drying process is carried out to precipitation;Institute
The condition for stating microwave radiation drying process is:Microwave radiation frequencies are 2450 ± 50MHz, and microwave radiation unit power is 0.50w/
G, microwave irradiation time 60min, microwave radiation temperature are 60 DEG C.
Remaining technological parameter and method with it is identical in embodiment 2.
Embodiment 10:
In the step 2, before cooling, reaction solution is added in stainless steel spherical container, spherical container is placed in four
On axle beveller, four axle bevellers are opened, drive stainless steel spherical container randomly to rotate, react 60min;The stainless steel is spherical
The charging aperture of container is sealed by threaded cap, and threaded cap flushes after being tightly connected with the surface of stainless steel spherical container;Described four
The active rotating speed of axle beveller is 150rpm, and stochastic transition frequency is 30s.
Remaining technological parameter and method with it is identical in embodiment 5.
Embodiment 11:
In the step 2, before cooling, reaction solution is added in stainless steel spherical container, spherical container is placed in four
On axle beveller, four axle bevellers are opened, drive stainless steel spherical container randomly to rotate, react 60min;The stainless steel is spherical
The charging aperture of container is sealed by threaded cap, and threaded cap flushes after being tightly connected with the surface of stainless steel spherical container;Described four
The active rotating speed of axle beveller is 150rpm, and stochastic transition frequency is 30s.
Remaining technological parameter and method with it is identical in embodiment 9.
Embodiment 12:
The drying is dried using microwave radiation, and its process is:Reactant after cleaning is put into quartzy drier, so
After be placed in microwave radiation reacting furnace;Nitrogen is passed through with 50mL/min speed, microwave radiation drying process is carried out to precipitation;Institute
The condition for stating microwave radiation drying process is:Microwave radiation frequencies are 2450 ± 50MHz, and microwave radiation unit power is 0.50w/
G, microwave irradiation time 60min, microwave radiation temperature are 60 DEG C.
Remaining technological parameter and method with it is identical in embodiment 5.
Embodiment 13:
The drying is dried using microwave radiation, and its process is:Reactant after cleaning is put into quartzy drier, so
After be placed in microwave radiation reacting furnace;Nitrogen is passed through with 50mL/min speed, microwave radiation drying process is carried out to precipitation;Institute
The condition for stating microwave radiation drying process is:Microwave radiation frequencies are 2450 ± 50MHz, and microwave radiation unit power is 0.50w/
G, microwave irradiation time 60min, microwave radiation temperature are 60 DEG C.
Remaining technological parameter and method with it is identical in embodiment 10.
The antibiotic property of the di copper sample of the preparation of embodiment 1~13 is examined using Escherichia coli (ATCC 8739).
Bacteria Culture is carried out using LB nutrient solutions.Using original bacterial suspension as a control group.It is used for using six parallel sampleses
Antibacterial tests.Each sample takes 10g di copper samples to be placed in 24 orifice plates, then takes 200 μ L bacterium solutions (106CFU/mL)
It is added to the surface of each sample.Then, in incubator 37 DEG C be incubated 12 hours, afterwards, take 800 milliliters of LB culture liquid to add
Enter, continue to be incubated at 37 DEG C 12 hours, finally, take 200 μ L bacteria suspensions of each sample and be transferred in 96 orifice plates.Bacterium
Grow through ELIASA (MQX200, BioTEK) detection (optical density, 600nm).
Table 1 shows the antibiotic rate for the di copper sample that the embodiment of the present invention 1~13 obtains;
Table 1
Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
Antibiotic rate | 48% | 72% | 70% | 80% | 82% | 78% | 77% |
Embodiment | 8 | 9 | 10 | 11 | 12 | 13 | |
Antibiotic rate | 75% | 74% | 86% | 80% | 84% | 90% |
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details and shown here as the legend with description.
Claims (10)
1. a kind of preparation method of antibiotic property hydroxyl cupric phosphate, it is characterised in that comprise the following steps:
Step 1: pressing parts by volume, the inorganic copper salt solution that 20~30 parts of mass fractions are 40~60% is added into 40~60 parts of matter
Measure in the acid-phosphate solution that fraction is 40~60%, stir 30~60min;Then NH is added3·H2O regulations pH to 2.5~
7;
Step 2: the solution after regulation pH is transferred into stainless steel cauldron, reacted 1~3 hour at 165~185 DEG C, it is cold
But, it is then centrifuged for, obtained solid is cleaned with deionized water, is dried, is obtained antibiotic property hydroxyl cupric phosphate.
2. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 1, it is characterised in that the inorganic copper salt solution
For any one in copper nitrate solution, copper chloride solution, copper-bath.
3. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 1, it is characterised in that the acid phosphate is molten
Liquid is in ammonium hydrogen phosphate solution, dibastic sodium phosphate solution, phosphoric acid hydrogen potassium solution, sodium dihydrogen phosphate, potassium dihydrogen phosphate
Any one.
4. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 1, it is characterised in that what the centrifugation used turns
Speed is 5000rpm, time 15min.
5. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 1, it is characterised in that the process of the step 1
Replace with:The inorganic copper salt solution that 20~30 parts of mass fractions are 40~60% is injected into the spray containers with stainless steel shower nozzle
In I and it is fixed on the propulsion pump I for being provided with high voltage electrostatic equipment;Simultaneously by 20~30 parts of mass fractions be 40~60% acid
Acid phosphate solution is injected into the spray containers II with stainless steel shower nozzle and is fixed on the propulsion for being provided with high voltage electrostatic equipment
On pump II;By weight, 1~5 part of surfactant is dissolved in the acid phosphate that 20~30 parts of mass fractions are 40~60%
Salting liquid, then insert in the reactor with agitating device;Utilized on the stainless steel syringe needle of spray containers I and spray containers II
High voltage electrostatic equipment sets high pressure, while sets the fltting speed for promoting pump I and promoting pump II, by inorganic copper salt solution and acid
Phosphate solution is instilled in reactor with drop state simultaneously;While drop instills reactor, stirring reaction, drop is added dropwise
After the completion of, continue 10~30min of stirring, ammonia is passed through into reactor while stirring, adjusts pH to 2.5~7.
6. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 5, it is characterised in that described stainless steel shower nozzle
Internal diameter be 0.5~1.2mm;Described propulsion pump I and the fltting speed of propulsion pump II are 15~20mL/h;High pressure size is 3-
8kV。
7. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 5, it is characterised in that the surfactant bag
Include the raw material of following parts by weight:5~10 parts of polyvinylpyrrolidones, 0.5~1 part of nonyl phenol, 0.3~0.5 part of 1- ethyl -3- first
Base imidazole lactic acid, 1~3 part of alkyl dimethyl betaine, 0.2~0.5 part of APG, 1~3 part of dodecyl dimethyl benzyl
Ammonium chloride.
8. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 1, it is characterised in that in the step 2,
Before cooling, reaction solution is added in stainless steel spherical container, spherical container is placed on four axle bevellers, open the grinding of four axles
Instrument, drive stainless steel spherical container randomly to rotate, react 30~60min;The charging aperture of the stainless steel spherical container passes through spiral shell
Line lid seals, and threaded cap flushes after being tightly connected with the surface of stainless steel spherical container;The driving shaft of the four axles beveller turns
Speed is 100~150rpm, and stochastic transition frequency is 10~30s.
9. the preparation method of antibiotic property hydroxyl cupric phosphate as claimed in claim 1, it is characterised in that the drying uses microwave
Radiant drying, its process are:Reactant after cleaning is put into quartzy drier, is subsequently placed in microwave radiation reacting furnace;
Nitrogen is passed through with 50~100mL/min speed, microwave radiation drying process is carried out to precipitation;The microwave radiation drying process
Condition be:Microwave radiation frequencies are 2450 ± 50MHz, and microwave radiation unit power is 0.10~1.00w/g, during microwave radiation
Between be 30~60min, microwave radiation temperature is 50~70 DEG C.
10. the antibiotic property hydroxyl cupric phosphate that a kind of preparation method as described in any one of claim 1~9 obtains is killing large intestine
Application in bacillus.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112644095A (en) * | 2020-12-24 | 2021-04-13 | 安徽品冠管业有限公司 | Antibacterial PP-R pipe and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103723756A (en) * | 2013-12-13 | 2014-04-16 | 绵阳市远达新材料有限公司 | Method for preparing strontium carbonate by utilizing high-voltage electrostatic field effect |
CN107226466A (en) * | 2017-08-01 | 2017-10-03 | 西南科技大学 | The method that nitrogen-doped graphene aeroge is prepared using plant extraction liquid modification |
-
2017
- 2017-10-16 CN CN201710958238.9A patent/CN107651659B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103723756A (en) * | 2013-12-13 | 2014-04-16 | 绵阳市远达新材料有限公司 | Method for preparing strontium carbonate by utilizing high-voltage electrostatic field effect |
CN107226466A (en) * | 2017-08-01 | 2017-10-03 | 西南科技大学 | The method that nitrogen-doped graphene aeroge is prepared using plant extraction liquid modification |
Non-Patent Citations (1)
Title |
---|
ZHANG HUI ET AL.: "Study of Photocatalytic Activities with Copper Hydroxyphosphate", 《MATERIALS SCIENCE FORUM VOLS》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112644095A (en) * | 2020-12-24 | 2021-04-13 | 安徽品冠管业有限公司 | Antibacterial PP-R pipe and preparation method thereof |
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CN107651659B (en) | 2020-04-07 |
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