CN104744880B - A kind of preparation method of phenolic resin carbonized zirconium suspension - Google Patents
A kind of preparation method of phenolic resin carbonized zirconium suspension Download PDFInfo
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- CN104744880B CN104744880B CN201510093305.6A CN201510093305A CN104744880B CN 104744880 B CN104744880 B CN 104744880B CN 201510093305 A CN201510093305 A CN 201510093305A CN 104744880 B CN104744880 B CN 104744880B
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- zirconium carbide
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Abstract
The present invention relates to a kind of preparation method of phenolic resin carbonized zirconium suspension, the preparation method of the phenolic resin carbonized zirconium suspension is：Phenolic resin is slowly added in organic solvent, it is sufficiently mixed with organic solvent and obtains phenol resin solution, it is slow added into dispersant, the zirconium carbide powder obtained after pretreatment is further slowly added to after stirring, the good phenolic resin carbonized zirconium suspension of standing stability is obtained through fully dispersed.The settling character of suspension is characterized by monitoring the change of suspension pressure, as a result shows that the suspension standing stability is good.
Description
Technical field
The present invention relates to a kind of preparation method of phenolic resin-zirconium carbide suspension and its standing characteristic present's method.
Background technology
Zirconium carbide (ZrC) belongs to typical face-centred cubic structure crystal, and Zr is similar to C lattice constant, and Zr atoms are formed
Close cubic lattice, and C atoms are in the octahedral interstice position of lattice.ZrC is with a variety of desirable physicals, chemical characteristic
One of important high-temperature structural material, such as ZrC has high-melting-point (3550 DEG C), and high rigidity (25GPa) is strong wear-resisting and corrosion-resistant
Property and high conductivity, ZrC these characteristics make it that it turns into all very promising material, such as knife in many application fields
Tool, wear parts, mechanical industry smelting furnace, especially because there is ZrC low neutron absorption cross-section and good radioresistance to cause
It is used for nuclear reactor core material.
ZrC powders are exactly to be added as functional additive in one of main application approach of fire-resistant oxidation resistant technical field
Into polymer composite, the purpose for improving composite high-temperature comprehensive property is reached.In order to realize this application, Wo Menbi
ZrC powders are exactly evenly dispersed in macromolecule solvent and form suspension liquid by the problem of need solving, and obtain high volume integral
Scattered macromolecule-ZrC powder (organic and inorganic) suspension of number, long-time stable, has resistance to meet some fields to figure layer surface
The requirement of high-temperature oxidation resistant.
The content of the invention
The technical problems to be solved by the invention are stood surely there is provided one kind for above shortcomings in the prior art
The preparation method of qualitative good phenolic resin-zirconium carbide suspension.
In order to solve the above technical problems, the technical scheme that the present invention is provided is：
A kind of preparation method of the good phenolic resin of standing stability-zirconium carbide suspension is provided, is specially：By phenolic aldehyde
Resin is slowly added in organic solvent, is sufficiently mixed with organic solvent and is obtained phenol resin solution, is slow added into dispersant, is stirred
The zirconium carbide powder obtained after pretreatment is further slowly added to after mixing uniformly, phenolic resin-carbonization is obtained through fully dispersed
Zirconium suspension.
By such scheme, phenolic resin solid content >=98%.
By such scheme, the organic solvent is acetone.
By such scheme, the dispersant is the BYK moist type dispersants that Bi Ke chemical companies of Germany produce.
By such scheme, the zirconium carbide powder pretreating process is：It is 35% by zirconium carbide powder and mass concentration
Concentrated hydrochloric acid in mass ratio 1:5 mixing, are stirred at room temperature 10h, then suction filtration, gained filter cake is washed with deionized to neutrality, and is dried
The zirconium carbide powder that dry, grinding is obtained after pretreatment；The zirconium carbide powder average grain diameter obtained after pretreatment
≤300nm。
By such scheme, the phenolic resin, organic solvent, dispersant, the zirconium carbide powder obtained after pretreatment
Mass ratio is 1:2:0.1~0.3:1.42.
Good phenolic resin-zirconium carbide the suspension of standing stability that the present invention is prepared according to the above method, institute
Suspension viscosity is stated less than 600mPas, 24h is stood without obvious delaminating deposition phenomenon.Hanged by monitoring phenolic resin-zirconium carbide
The change of turbid hydraulic pressure by force characterizes the settling character of suspension, is specially：Phenolic resin-zirconium carbide suspension is positioned over a circle
In column type container, pressure sensor, the liquid layer pressure of pressure sensor detection suspension at the middle and upper levels are provided with the middle and upper part of container
By force, the lamination of pressure sensor collection liquid it is strong at intervals of 30s once, acquisition time is 24h, according to the change of suspension pressure come
Reflect the Deposition Characteristic of solid phase particles in suspension.
The present invention principle be：The present invention adds moist type macromolecule in phenolic resin-zirconium carbide suspension and disperseed
Agent, the addition of macromolecule dispersing agent can make ZrC powder produce steric hindrance effect in liquid phase phenolic resin, so as to be beneficial to
Improve the stability of suspension.Use the powder pre-treating technique of chlorohydric acid pickling ZrC powder, thus it is possible to vary ZrC particle surfaces
State of charge and pH value, improve steric hindrance effect of the ZrC powder in liquid phase phenolic resin, so as to improve the stabilization of suspension
Property.
The present invention characterizes suspension within this period of time using the method for detection suspension middle and upper part liquid layer pressure change
Standing characteristic.For the liquid layer of a certain determination height, the factor of this layer of liquid pressure is influenceed there was only the density of this layer of liquid, institute
With the change by detecting this layer of liquid pressure, the change of this layer of fluid density is obtained, and then symbolizes suspension at this section
Interior standing characteristic.
The beneficial effects of the present invention are：By ZrC powder being pre-processed and being added suitable dispersant, increase
ZrC and phenolic resin compatibility, proportion optimizing are finally prepared the PF-ZrC with good fluidity and standing stability and hanged
Turbid liquid.
Brief description of the drawings
Fig. 1 is the viscosity profile of the PF-ZrC suspensions standing different time prepared by embodiment 1；
Fig. 2 is that liquid layer stands pressure in 24h and changed with time song at the middle and upper levels for PF-ZrC suspensions prepared by embodiment 1
Line；
Fig. 3 is that liquid layer stands pressure in 24h and changed with time song at the middle and upper levels for PF-ZrC suspensions prepared by embodiment 2
Line；
Fig. 4 is that liquid layer stands pressure in 24h and changed with time song at the middle and upper levels for PF-ZrC suspensions prepared by embodiment 3
Line；
Fig. 5 is that liquid layer stands pressure in 24h and changed with time song at the middle and upper levels for PF-ZrC suspensions prepared by embodiment 4
Line；
Fig. 6 is that liquid layer stands pressure in 24h and changed with time song at the middle and upper levels for PF-ZrC suspensions prepared by embodiment 5
Line.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made below in conjunction with the accompanying drawings into
One step is described in detail.
Dispersant used by the embodiment of the present invention is the BYK moist type dispersants that Bi Ke chemical companies of Germany produce.
Embodiment 1
Zirconium carbide powder is pre-processed：By the concentrated hydrochloric acid in mass ratio 1 that zirconium carbide powder and mass concentration are 35%:5 mixing,
10h is stirred at room temperature, then suction filtration, gained filter cake is washed with deionized to neutrality, and dries, grind and obtain after pretreatment
The zirconium carbide powder arrived, average grain diameter is 300nm.
By 5 grams of phenolic resin, (PF, solid content >=98%) be slowly added in 10g acetone, stirring 3h obtains PF solution, and PF is molten
Liquid is while be stirred at room temperature, while being slowly dropped into dispersant, dropwise addition 1.5g dispersants, stir another side stirring one side after 2h altogether
The ZrC powder obtained after pretreatment is slowly added to, is obtained after the ZrC powder that 7.1g is obtained after pretreatment, stirring 3h are added altogether
Obtain PF-ZrC suspensions.
After tested, the suspended fluid viscosities of PF-ZrC manufactured in the present embodiment are 212mPas, and mobility is preferable.
In the suspension pressure test device that PF-ZrC suspensions are positioned over to cylinder, the device is set in the middle part of container
Pressure sensor is equipped with, detect the liquid layer pressure of suspension at the middle and upper levels by pressure sensor settles situation to monitor suspension,
The lamination of pressure sensor collection liquid it is strong at intervals of 30s once, acquisition time is 24h.
The PF-ZrC suspensions prepared by the present embodiment stand the viscosity profile of different time as shown in Figure 1, from figure
In can show that in Each point in time viscosity B coefficent fluctuation is little, illustrate that ZrC-PF suspension standing stabilities are good.Fig. 2 is
Liquid layer stands pressure versus time curve in 24h to PF-ZrC suspensions prepared by the present embodiment at the middle and upper levels, from figure
Go out 0.7232Pa of the liquid layer pressure from beginning, drop to 0.6512Pa after standing 24h, pressure change is 10%, illustrates suspension
Standing in 24h, liquid layer is without obvious pressure change, and the standing stability of suspension is good.
Embodiment 2
Zirconium carbide powder is pre-processed：By the concentrated hydrochloric acid in mass ratio 1 that zirconium carbide powder and mass concentration are 35%:5 mixing,
10h is stirred at room temperature, then suction filtration, gained filter cake is washed with deionized to neutrality, and dries, grind and obtain after pretreatment
The zirconium carbide powder arrived, average grain diameter is 300nm.
By 5 grams of phenolic resin, (PF, solid content >=98%) be slowly added in 10g acetone, stirring 3h obtains PF solution, and PF is molten
Liquid is while be stirred at room temperature, while being slowly dropped into dispersant, dropwise addition 0.5g dispersants, stir another side stirring one side after 2h altogether
Pretreated ZrC powder is slowly added to, acquisition PF-ZrC after the pretreated ZrC powder of 7.1g, stirring 3h is added altogether suspended
Liquid.
After tested, the suspended fluid viscosities of PF-ZrC manufactured in the present embodiment are 521mPas, and mobility is preferable.
PF-ZrC suspensions are positioned in suspension pressure test device, the suspension pressure change is illustrated in figure 3
Curve, it is 18.3% standing pressure change in 24h that suspension is drawn from curve, illustrates that the PF-ZrC suspensions are stood stable
Property is preferable.
Embodiment 3
Zirconium carbide powder is pre-processed：By the concentrated hydrochloric acid in mass ratio 1 that zirconium carbide powder and mass concentration are 35%:5 mixing,
10h is stirred at room temperature, then suction filtration, gained filter cake is washed with deionized to neutrality, and dries, grind and obtain after pretreatment
The zirconium carbide powder arrived, average grain diameter is 300nm.
By 5 grams of phenolic resin, (PF, solid content >=98%) be slowly added in 10g acetone, stirring 3h obtains PF solution, and PF is molten
Liquid is while be stirred at room temperature, while being slowly added to the ZrC powder obtained after pretreatment, adds 6.45g after pretreatment altogether
PF-ZrC suspensions are obtained after obtained ZrC powder, stirring 3h.
After tested, the suspended fluid viscosities of PF-ZrC manufactured in the present embodiment are 1.51Pas, poor fluidity.
PF-ZrC suspensions are positioned in suspension pressure test device, the suspension pressure change is illustrated in figure 4
Curve, it is 43.4% standing pressure change in 24h that suspension is drawn from curve, illustrates that the PF-ZrC suspensions are stood stable
Property is poor.
Embodiment 4
Zirconium carbide powder is pre-processed：By the concentrated hydrochloric acid in mass ratio 1 that zirconium carbide powder and mass concentration are 35%:5 mixing,
10h is stirred at room temperature, then suction filtration, gained filter cake is washed with deionized to neutrality, and dries, grind and obtain after pretreatment
The zirconium carbide powder arrived, average grain diameter is 300nm.
By 5 grams of phenolic resin, (PF, solid content >=98%) be slowly added in 10g acetone, stirring 3h obtains PF solution, and PF is molten
Liquid is while be stirred at room temperature, while being slowly dropped into dispersant, dropwise addition 2.5g dispersants, stir another side stirring one side after 2h altogether
The ZrC powder obtained after pretreatment is slowly added to, is obtained after the ZrC powder that 7.1g is obtained after pretreatment, stirring 3h are added altogether
Obtain PF-ZrC suspensions.
After tested, the suspended fluid viscosities of PF-ZrC manufactured in the present embodiment are 1.6Pas, poor fluidity.
PF-ZrC suspensions are positioned in suspension pressure test device, suspension pressure change is illustrated in figure 5
Change curve, it is 26.1% standing pressure change in 24h that suspension is drawn from curve, illustrates that the PF-ZrC suspensions are stood steady
It is qualitative poor.
Embodiment 5
By 5 grams of phenolic resin, (PF, solid content >=98%) be slowly added in 10g acetone, stirring 3h obtains PF solution, and PF is molten
Liquid is while be stirred at room temperature, while being slowly dropped into dispersant, dropwise addition 1.5g dispersants, stir another side stirring one side after 2h altogether
Not pretreated ZrC powder is slowly added to, PF-ZrC is obtained after the not pretreated ZrC powder of 7.1g, stirring 3h are added altogether
Suspension.
After tested, the suspended fluid viscosities of PF-ZrC manufactured in the present embodiment are 952mPas, and mobility is poor.
PF-ZrC suspensions are positioned in suspension pressure test device, the suspension pressure change is illustrated in figure 6
Curve, it is 29.3% standing pressure change in 24h that suspension is drawn from curve, illustrates that the PF-ZrC suspensions are stood stable
Property is poor.
Claims (3)
1. a kind of preparation method of the good phenolic resin of standing stability-zirconium carbide suspension, it is characterised in that：By phenolic aldehyde tree
Fat is slowly added in organic solvent, is sufficiently mixed with organic solvent and is obtained phenol resin solution, is slow added into dispersant, stirring
The zirconium carbide powder obtained after pretreatment is further slowly added to after uniform, phenolic resin-zirconium carbide is obtained through fully dispersed
Suspension；
The organic solvent is acetone；
The dispersant is the BYK moist type dispersants that Bi Ke chemical companies of Germany produce；
The zirconium carbide powder pretreating process is：By the concentrated hydrochloric acid in mass ratio 1 that zirconium carbide powder and mass concentration are 35%:
5 mixing, 10h is stirred at room temperature, then suction filtration, gained filter cake is washed with deionized to neutrality, and dry, grind obtain through in advance locate
The zirconium carbide powder obtained after reason；Zirconium carbide powder average grain diameter≤the 300nm obtained after pretreatment；
The phenolic resin, organic solvent, dispersant, the mass ratio of the zirconium carbide powder obtained after pretreatment are 1:2:0.1
~0.3:1.42.
2. the preparation method of the good phenolic resin of standing stability according to claim 1-zirconium carbide suspension, it is special
Levy and be：Phenolic resin solid content >=98%.
3. the good phenolic resin of a kind of standing stability-zirconium carbide suspension, it is characterised in that appointed according to claim 1-2
One methods described is prepared, and the suspended fluid viscosity is less than 600mPas, stands 24h without obvious delaminating deposition phenomenon.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774580A (en) * | 2010-01-25 | 2010-07-14 | 武汉理工大学 | Method for purifying zirconium carbide powder |
| CN103788727A (en) * | 2012-11-02 | 2014-05-14 | 中冶建筑研究总院有限公司 | Protective paint for steel structure surface and preparation method thereof |
| CN103806267A (en) * | 2013-12-21 | 2014-05-21 | 中国科学院上海硅酸盐研究所 | Method for preparing zirconium carbide ceramic boundary phase on surface of carbon fiber |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2333888C1 (en) * | 2007-04-06 | 2008-09-20 | Московская государственная академия тонкой химической технологии им. М.В. Ломоносова | Method for obtaining highly-dispersible refractory carbides for coating and composites based thereon |
| CN102887709A (en) * | 2012-11-05 | 2013-01-23 | 中国人民解放军国防科学技术大学 | ZrC (Zirconium Carbide) ceramic precursor, ZrC ceramic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774580A (en) * | 2010-01-25 | 2010-07-14 | 武汉理工大学 | Method for purifying zirconium carbide powder |
| CN103788727A (en) * | 2012-11-02 | 2014-05-14 | 中冶建筑研究总院有限公司 | Protective paint for steel structure surface and preparation method thereof |
| CN103806267A (en) * | 2013-12-21 | 2014-05-21 | 中国科学院上海硅酸盐研究所 | Method for preparing zirconium carbide ceramic boundary phase on surface of carbon fiber |
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