CN107359346A - A kind of anode material of lithium battery modified multicomponent presoma and preparation method - Google Patents
A kind of anode material of lithium battery modified multicomponent presoma and preparation method Download PDFInfo
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- CN107359346A CN107359346A CN201710463591.XA CN201710463591A CN107359346A CN 107359346 A CN107359346 A CN 107359346A CN 201710463591 A CN201710463591 A CN 201710463591A CN 107359346 A CN107359346 A CN 107359346A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention is applied to presoma manufacturing technology field, a kind of anode material of lithium battery modified multicomponent presoma is provided, the presoma includes kernel, intermediate layer and outer shell, it is First Transition layer wherein between kernel and intermediate layer, it is the second transition zone between intermediate layer and shell, the First Transition layer is the concentration gradient transition material from material contained by material to intermediate layer contained by kernel, and second transition zone is the concentration gradient transition material from material contained by material to outer shell contained by intermediate layer.The present invention is changed by the elemental composition and concentration of element for rationally setting each layer, and when precursor is used as anode material for lithium-ion batteries, compared with common tertiary cathode material, good cycling stability, specific capacity are high, more suitable for the application of electrokinetic cell.
Description
Technical field
The invention belongs to presoma manufacturing technology field, more particularly to a kind of anode material of lithium battery modified multicomponent presoma
And preparation method.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, and important function is increasingly shown in every field.As lithium
The important component of ion battery, the positive electrode of lithium battery decide the performance of lithium battery, price and development.
Current all kinds of anode material for lithium-ion batteries common are cobalt acid lithium (LCO), nickle cobalt lithium manganate (NCM), LiMn2O4
(LMO), LiFePO4 (LFP), nickel cobalt lithium aluminate (NCA) etc., wherein nickel cobalt aluminium tertiary cathode material are because cost of material is low, tool
There are higher specific capacity and stable circulation performance and turn into the focus of recent research.Although but current nickel cobalt manganese anode material
Specific capacity is high, but the activity and cyclical stability of material are poor, and particularly heat-resisting ability is also relatively weak.
The content of the invention
In view of the above problems, it is an object of the invention to provide a kind of anode material of lithium battery modified multicomponent presoma and system
Preparation Method, it is intended to solve the technical problem that existing anode material of lithium battery is active, cyclical stability and heat-resisting ability are poor.
On the one hand, the anode material of lithium battery modified multicomponent presoma, including kernel, intermediate layer and outer shell, wherein
It is First Transition layer between kernel and intermediate layer, is the second transition zone between intermediate layer and shell, wherein;
The kernel contains Ni and Mn elements, and mol ratio Ni:Mn=1:(1.2-2);
Ni, Co, Mn element are contained in the intermediate layer, and wherein Co constituent contents are more than 1/3 and towards outer shell direction content
Gradually rise, and Ni with Mn constituent contents are identical, and gradually reduced towards outer shell direction content;
The outer shell contains Ni, Co, Al element, and mol ratio Ni:Co:Al=1:(1-1.4):(0.3-0.5), wherein
Content towards outer shell surface direction Ni and Co gradually reduces, and Al content gradually rises;
The First Transition layer is the concentration gradient transition material from material contained by material to intermediate layer contained by kernel, described
Second transition zone is the concentration gradient transition material from material contained by material to outer shell contained by intermediate layer.
Further, a diameter of 5-11 microns of the kernel, the thickness in the intermediate layer are 2-5 microns, the shell
The thickness of layer is 2-5 microns.
Further, the thickness of the one the second transition zones is 0.5-1 microns.
On the other hand, the preparation method of the anode material of lithium battery modified multicomponent presoma, comprises the steps:
Prepare kernel step:According to mol ratio Ni:Mn=1:(1.2-2) configures the violent mixing salt solution X of nickel, and it is molten to prepare highly basic
Liquid, solution X and strong base solution are added to reaction vessel with certain speed and are stirred carry out coprecipitation reaction, obtained precipitation
Thing is kernel;
Prepare First Transition layer step:Nickel cobalt manganese mixing salt solution Y is configured, wherein Co constituent contents are more than 1/3, Ni and Mn
Constituent content is identical, continues into the reaction vessel to be gradually added solution X with decline rate, while with increasing velocity to described
Solution Y is synchronously added in reaction vessel, while adjustment strong base solution addition speed so that the surface of the kernel after
Continuous accumulation precipitation, forms First Transition layer;
Prepare intermediate layer step:The cobalt salt mixed solution Z and violent salting liquid W of nickel is configured, the violent elemental mole ratios example of nickel in solution W
It is identical, when solution X, which adds speed, reduces to zero, while stop adding solution Y, then synchronously add the solution Z that has configured and molten
Liquid W, wherein solution Z addition speed gradually increase, and the addition speed of solution W is gradually reduced, and the solution Z and solution added
Need to keep wherein Co constituent contents to be more than the 1/3 of total addition during W, the addition speed of strong base solution is adjusted during this, with
Make to continue accumulation precipitation on the surface of a transition zone, form intermediate layer;
Prepare the second transition layer process:Configure nickel cobalt aluminium mixing salt solution M, wherein mol ratio Ni:Co:Al=1:(1-
1.4):(0.3-0.5), Solutions Solution Y is gradually added into the reaction vessel with decline rate, while with increasing velocity to institute
State and solution M is synchronously added in reaction vessel, while the addition speed of adjustment strong base solution, so that the table in the intermediate layer
Accumulation precipitation is continued in face, forms the second transition zone;
Prepare outer shell step:Nickel cobalt mixed salt solution N and aluminum salt solution P is configured, zero is reduced to when solution Y adds speed
When, while stop adding solution M, the solution N and solution P configured is then synchronously added, wherein solution P addition speed is gradual
Increase, solution N addition speed are gradually reduced, and need to keep mol ratio Ni when the solution P and solution N of addition:Co:Al=
1:(1-1.4):(0.3-0.5), during this adjust strong base solution addition speed so that the surface of two transition zone after
Continuous accumulation precipitation, forms outer shell;
Solid-liquid separation step:After the completion of outer shell deposition, the solution in reaction vessel is separated by filtration, presoma is collected and sinks
Product thing, and dry.
Further, in above-mentioned each step, when adjusting the addition speed of strong base solution, need to keep in reaction vessel
PH value is 9.5-11.5.
The beneficial effects of the invention are as follows:Anode material of lithium battery modified multicomponent presoma provided by the invention is altogether by five layers
Composition, respectively kernel, First Transition layer, intermediate layer, the second transition zone and outer shell, the wherein effective element of inner nuclear layer is manganese
And nickel, the effective element in intermediate layer is nickel cobalt manganese, and the effective element of outer shell is nickel cobalt aluminium, and First Transition layer is from kernel
The concentration gradient transition material of material contained by contained material to intermediate layer, second transition zone be from material contained by intermediate layer to
The concentration gradient transition material of material contained by outer shell, changed by the elemental composition and concentration of element that rationally set each layer,
When precursor is used as anode material for lithium-ion batteries, compared with common tertiary cathode material, good cycling stability, specific capacity
Height, more suitable for the application of electrokinetic cell.
Brief description of the drawings
Fig. 1 is the sectional structure chart of anode material of lithium battery modified multicomponent presoma provided in an embodiment of the present invention;
Fig. 2 is the flow chart provided in an embodiment of the present invention for preparing anode material of lithium battery modified multicomponent presoma;
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
In order to illustrate technical solutions according to the invention, illustrated below by specific embodiment.
Fig. 1 shows the structure of anode material of lithium battery modified multicomponent presoma provided in an embodiment of the present invention, in order to just
The part related to the embodiment of the present invention is illustrate only in explanation.
As shown in figure 1, the anode material of lithium battery modified multicomponent presoma, is followed successively by kernel 1, the first mistake from the inside to the outside
Layer 2, intermediate layer 3, the second transition zone 4 and outer shell 5 are crossed, wherein;
The kernel contains Ni and Mn elements, and mol ratio Ni:Mn=1:(1.2-2);
Ni, Co, Mn element are contained in the intermediate layer, and wherein Co constituent contents are more than 1/3 and towards outer shell direction content
Gradually rise, and Ni with Mn constituent contents are identical, and gradually reduced towards outer shell direction content;
The outer shell contains Ni, Co, Al element, and mol ratio Ni:Co:Al=1:(1-1.4):(0.3-0.5), wherein
Content towards outer shell surface direction Ni and Co gradually reduces, and Al content gradually rises;
The First Transition layer is the concentration gradient transition material from material contained by material to intermediate layer contained by kernel, described
Second transition zone is the concentration gradient transition material from material contained by material to outer shell contained by intermediate layer.
In foregoing description, kernel is the violent hydroxide of nickel, and intermediate layer is nickel cobalt manganese hydroxide, and outer shell is nickel cobalt aluminium hydrogen
Oxide.And need to control Ni in kernel:Mn mol ratio=1:(1.2 to 2);Co constituent contents are more than 1/3, Ni in intermediate layer
It is identical with Mn constituent contents;Ni in outer shell:Co:Al mol ratio=1:(1 to 1.4):(0.3 to 0.5).And in intermediate layer and
Content towards outer shell direction Ni and Mn gradually reduces;It is equal towards outer shell surface direction Ni and Co content in outer shell
Gradually reduce, Al content gradually rises.
For said structure, the embodiment of the present invention additionally provides a kind of system of anode material of lithium battery modified multicomponent presoma
Preparation Method, as shown in Fig. 2 comprising the steps:
S101, prepare kernel step.
According to mol ratio Ni:Mn=1:(1.2-2) configures the violent mixing salt solution X of nickel, prepares strong base solution, by solution X and
Strong base solution is added to reaction vessel with certain speed and is stirred carry out coprecipitation reaction, and obtained sediment is kernel,
The interior nuclear diameter typically deposited is to 5-11 microns, it usually needs reaction 10-20 hours.
S102, prepare First Transition layer step.
Nickel cobalt manganese mixing salt solution Y is configured, wherein Co constituent contents are identical more than 1/3, Ni and Mn constituent contents, to successively decrease
Speed continues to be gradually added solution X into the reaction vessel, while is synchronously added into the reaction vessel with increasing velocity
Solution Y, while the addition speed of adjustment strong base solution, so as to continue accumulation precipitation on the surface of the kernel, forms the
One transition zone, First Transition thickness degree are 0.5-1 microns, probably need to react half an hour to 1 hour.
S103, prepare intermediate layer step.
The cobalt salt mixed solution Z and violent salting liquid W of nickel is configured, the violent elemental mole ratios example of nickel is identical in solution W, when solution X adds
When entering speed and reducing to zero, while stop adding solution Y, then synchronously add the solution Z configured and solution W, wherein solution Z's
Adding speed gradually increases, and the addition speed of solution W is gradually reduced, and needs to keep wherein when the solution Z and solution W of addition
Co constituent contents are more than the 1/3 of total addition, the addition speed of strong base solution are adjusted during this, so that in a transition zone
Surface continue accumulation precipitation, formed intermediate layer;The intermediate layer thickness is 2-5 microns, it is necessary to react 4-10 hours.
S104, prepare the second transition layer process.
Configure nickel cobalt aluminium mixing salt solution M, wherein mol ratio Ni:Co:Al=1:(1-1.4):(0.3-0.5), to successively decrease
Speed is gradually added Solutions Solution Y into the reaction vessel, while is synchronously added into the reaction vessel with increasing velocity
Solution M, while the addition speed of adjustment strong base solution, so as to continue accumulation precipitation on the surface in the intermediate layer, is formed
Second transition zone;Need to react half an hour to 1 hour, thickness is 0.5-1 microns.
S105, prepare outer shell step.
Nickel cobalt mixed salt solution N and aluminum salt solution P is configured, when solution Y, which adds speed, reduces to zero, while stops adding molten
Liquid M, the solution N and solution P configured is then synchronously added, wherein solution P addition speed gradually increases, solution N addition
Speed is gradually reduced, and needs to keep mol ratio Ni when the solution P and solution N of addition:Co:Al=1:(1-1.4):(0.3-
0.5) the addition speed of strong base solution, is adjusted during this, so as to continue accumulation precipitation on the surface of two transition zone, is formed
Outer shell, the outer shell thickness are 2-5 microns, it is necessary to react 4-10 hours.
S106, solid-liquid separation step.
After the completion of outer shell deposition, the solution in reaction vessel is separated by filtration, collects presoma deposit, and dry.
A specific embodiment is set forth below.
According to mol ratio Ni:Mn=1:1.5 configuration nickel violent mixing salt solution X, total concentration 1mol/L, prepare strong base solution
NaOH and ammoniacal liquor, solution X is added to reaction vessel with 150L/h speed, and synchronously add strong base solution and be stirred progress
Coprecipitation reaction, the pH value in reaction vessel is controlled between 9.5-10.5, obtained sediment is kernel, and reaction 17 is small
When.
Configure nickel cobalt manganese mixing salt solution Y, wherein Co constituent contents are half, Ni and Mn constituent contents everybody four/
One, total concentration 1.5mol/L.The decline rate for having 150L/h to zero in one hour continues progressively into the reaction vessel
Solution X is added, while solution Y is synchronously added into the reaction vessel with the increasing velocity in one hour from 0 to 130L/h, and
And the addition speed of strong base solution is adjusted simultaneously so that the pH value in reaction vessel is between 9.5-10.5, so that described interior
Accumulation precipitation is continued on the surface of core, forms First Transition layer, reacts 1 hour.
The cobalt salt mixed solution Z and violent salting liquid W of nickel is configured, the violent elemental mole ratios example of nickel is identical in solution W, in solution Z
Cobalt element concentration is the violent concentration of element sum of nickel in solution W, is 1.5mol/L.After the completion of the generation of First Transition layer, stop adding
Solution Y, the solution Z configured and solution W are then synchronously added, wherein solution Z addition speed gradually increases, and solution W adds
Enter speed to be gradually reduced, it is 120L/h, amplitude of variation 5L/h to add initial velocity, and it is 8 hours to add the reaction time altogether,
And the solution Z that adds and need during solution W to keep wherein Co constituent contents to be more than the 1/3 of total addition, adjust during this
The addition speed of strong base solution so that the pH value in reaction vessel is between 9.5-10.5, so that in the table of a transition zone
Accumulation precipitation is continued in face, forms intermediate layer.
Configure nickel cobalt aluminium mixing salt solution M, total concentration 1.5mol/L, wherein mol ratio Ni:Co:Al=1:1.2:0.4,
Decline rate from 130L/h to 0 within a hour is gradually added Solutions Solution Y into the reaction vessel, while small with one
When it is interior solution M is synchronously added into the reaction vessel from 0 to 150L/h increasing velocities, while adjustment strong base solution plus
Entering speed so that the pH value in reaction vessel is between 9.5-10.5, so as to continue accumulation precipitation on the surface in the intermediate layer,
Form the second transition zone;Reaction time is 1 hour.
Nickel cobalt mixed salt solution N and aluminum salt solution P is configured, is 1.5mol/L, when solution Y, which adds speed, reduces to zero,
Second transition zone is completely formed, while stops adding solution M, is then synchronously added the solution N and solution P configured, is added just
Beginning speed is 120L/h, and wherein solution P addition speed gradually increases, and solution N addition speed is gradually reduced, amplitude of variation
For 5L/h, and add solution P and solution N when need to keep mol ratio Ni:Co:Al=1:(1-1.4):(0.3-0.5), this
During adjust strong base solution addition speed so that continue on the surface of two transition zone accumulation precipitation, formed outer shell,
Need reaction 7 hours.
After the completion of outer shell deposition, the solution in reaction vessel is separated by filtration, collects presoma deposit, and is dried,
Final nickel cobalt manganese aluminium hydroxide presoma is obtained, nickel cobalt manganese lithium aluminate cathode material is then made, is finally made power electric
Pond.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (5)
- A kind of 1. anode material of lithium battery modified multicomponent presoma, it is characterised in that the presoma include kernel, intermediate layer and It is First Transition layer between outer shell, wherein kernel and intermediate layer, is the second transition zone between intermediate layer and shell, wherein;The kernel contains Ni and Mn elements, and mol ratio Ni:Mn=1:(1.2-2);Ni, Co, Mn element are contained in the intermediate layer, and wherein Co constituent contents are more than 1/3 and gradual towards outer shell direction content Rise, and Ni with Mn constituent contents are identical, and gradually reduced towards outer shell direction content;The outer shell contains Ni, Co, Al element, and mol ratio Ni:Co:Al=1:(1-1.4):(0.3-0.5), wherein towards Outer shell surface direction Ni and Co content gradually reduce, and Al content gradually rises;The First Transition layer is from the concentration gradient transition material of material contained by material to intermediate layer contained by kernel described second Transition zone is the concentration gradient transition material from material contained by material to outer shell contained by intermediate layer.
- 2. anode material of lithium battery modified multicomponent presoma as claimed in claim 1, it is characterised in that the kernel it is a diameter of 5-11 microns, the thickness in the intermediate layer is 2-5 microns, and the thickness of the outer shell is 2-5 microns.
- 3. anode material of lithium battery modified multicomponent presoma as claimed in claim 2, it is characterised in that the one the second transition zones Thickness is 0.5-1 microns.
- 4. a kind of preparation method of anode material of lithium battery modified multicomponent presoma, it is characterised in that methods described includes following Step:Prepare kernel step:According to mol ratio Ni:Mn=1:(1.2-2) configures the violent mixing salt solution X of nickel, prepares strong base solution, Solution X and strong base solution are added to reaction vessel with certain speed and are stirred carry out coprecipitation reaction, obtained sediment As kernel;Prepare First Transition layer step:Nickel cobalt manganese mixing salt solution Y is configured, wherein Co constituent contents are more than 1/3, Ni and Mn elements Content is identical, continues into the reaction vessel to be gradually added solution X with decline rate, while with increasing velocity to the reaction Solution Y is synchronously added in container, while the addition speed of adjustment strong base solution, so as to continue to accumulate on the surface of the kernel Tired precipitation, forms First Transition layer;Prepare intermediate layer step:The cobalt salt mixed solution Z and violent salting liquid W of nickel is configured, the violent elemental mole ratios example phase of nickel in solution W Together, when solution X, which adds speed, reduces to zero, while stop adding solution Y, then synchronously add the solution Z and solution configured W, wherein solution Z addition speed gradually increase, and the addition speed of solution W is gradually reduced, and the solution Z and solution W added When need keep wherein Co constituent contents be more than total addition 1/3, during this adjust strong base solution addition speed so that Continue accumulation precipitation on the surface of a transition zone, form intermediate layer;Prepare the second transition layer process:Configure nickel cobalt aluminium mixing salt solution M, wherein mol ratio Ni:Co:Al=1:(1-1.4): (0.3-0.5), Solutions Solution Y is gradually added into the reaction vessel with decline rate, while with increasing velocity to described anti- Answer and solution M synchronously added in container, while adjustment strong base solution addition speed so that the surface in the intermediate layer after Continuous accumulation precipitation, forms the second transition zone;Prepare outer shell step:Nickel cobalt mixed salt solution N and aluminum salt solution P is configured, when solution Y, which adds speed, reduces to zero, together When stop add solution M, then synchronously add the solution N and solution P configured, wherein solution P addition speed gradually increases, Solution N addition speed is gradually reduced, and needs to keep mol ratio Ni when the solution P and solution N of addition:Co:Al=1:(1- 1.4):(0.3-0.5), the addition speed of strong base solution is adjusted during this, so as to continue to accumulate on the surface of two transition zone Tired precipitation, forms outer shell;Solid-liquid separation step:After the completion of outer shell deposition, the solution in reaction vessel is separated by filtration, collects presoma deposition Thing, and dry.
- 5. the preparation method of anode material of lithium battery modified multicomponent presoma as claimed in claim 4, it is characterised in that above-mentioned each In individual step, when adjusting the addition speed of strong base solution, it is 9.5-11.5 that need to keep the pH value in reaction vessel.
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