CN105617934B - Hexagonal boron nitride dispersant and process for dispersing - Google Patents
Hexagonal boron nitride dispersant and process for dispersing Download PDFInfo
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- CN105617934B CN105617934B CN201510995199.0A CN201510995199A CN105617934B CN 105617934 B CN105617934 B CN 105617934B CN 201510995199 A CN201510995199 A CN 201510995199A CN 105617934 B CN105617934 B CN 105617934B
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- boron nitride
- hexagonal boron
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Abstract
The invention provides a kind of hexagonal boron nitride dispersant, wherein, it includes the component of following mass percent：Alkyl anion surfactant 8.0% 10.0%, the unrighted acids of C16 18 4.0% 6.0%, carboxymethyl cellulose 3.0% 5.0%, NPE 2.0% 4.0%, fatty acid ethanol amide 2.0 4.0%, ethoxylation sodium sulfonate 1.0% 3.0%, N, N are double（Polyoxyethylene）Alkylamine N oxides 0.5% 1.5%, sodium hydroxide 0.5% 1.5%, remaining is pure water.The present invention also provides a kind of process for dispersing of hexagonal boron nitride, and this method utilizes above-mentioned hexagonal boron nitride dispersant hexagonal boron nitride.Each component in the hexagonal boron nitride dispersant that the present invention is provided cooperates, and cooperates, hexagonal boron nitride powder can be caused equably, stably to disperse, it is to avoid or reduce the possibility reunited.
Description
Technical field
The present invention relates to a kind of dispersant and process for dispersing with graphite laminate structural material, more particularly to a kind of six side
Nitrogenize borated dispersant and process for dispersing.
Background technology
The crystal structure of hexagonal boron nitride has similar graphite laminate structure, and loose, lubrication, the easy moisture absorption, light weight is presented
Etc. the white powder of character, with good electrical insulating property, thermal conductivity, chemical stability, no sharp melting point.It is to prepare cube
The main raw material(s) of boron nitride, the detection of its granularity and pattern is extremely important.
But hexagonal boron nitride cold water insoluble, adding water, hydrolysis is very slow when boiling and produces a small amount of boric acid and ammonia, with
Weak acid and highly basic equal Fails To Respond at room temperature.Conventional silicic acid dipersant is undesirable to its peptizaiton, detection granularity and
Easily occur bimodal during distribution, and detection granularity, size distribution and true granularity, size distribution have deviation.In addition, common is scattered
The scattered hexagonal boron nitride micro mist of agent may pollute laser particle size analyzer sample cell, cause high background, it is necessary to repeatedly big
Measure pure water and rinse sample cell, this all brings very burden to actual production.
The content of the invention
In view of this, the present invention is above-mentioned to solve it is necessory to provide a kind of hexagonal boron nitride dispersant and process for dispersing
Problem.
Specifically, the present invention provides a kind of hexagonal boron nitride dispersant, and it includes the component of following mass percent：Alkyl
Anion surfactant 8.0%-10.0%, C16-18 unrighted acid 4.0%-6.0%, carboxymethyl cellulose 3.0%-5.0%,
NPE 2.0%-4.0%, fatty acid ethanol amide 2.0-4.0%, ethoxylation sodium sulfonate 1.0%-3.0%, N, N-
It is double（Polyoxyethylene）Alkyl amine n-oxide 0.5%-1.5%, sodium hydroxide 0.5%-1.5%, remaining is pure water.
Wherein, " alkyl anion surfactant " herein refers to the anion surfactant containing alkyl；This
" C16-18 unrighted acids " in text refers to the unsaturated lipid containing 16-18 carbon atom and containing carbon-carbon double bond or three key
Fat acid.
Based on above-mentioned, the alkyl anion surfactant be sodium alkyl benzene sulfonate, lauryl sodium sulfate or its
Meaning combination.
The present invention also provides a kind of process for dispersing of hexagonal boron nitride, and it comprises the following steps：
Mixing is stood：0.015-0.080 g hexagonal boron nitrides micro mist, 0.5-2 ml dispersion liquid and pure water are mixed,
And sealing and standing 36-72 hours, the pre-dispersed system of hexagonal boron nitride is obtained, wherein, the dispersion liquid is by above-mentioned hexagonal boron nitride
Dispersant and the pure water of dilution composition；
Ultrasonic vibration：Using the pre-dispersed system of hexagonal boron nitride described in ultrasonic oscillation, stable point of hexagonal boron nitride is obtained
Granular media system.
Based on above-mentioned, in the dispersion liquid, the body of the hexagonal boron nitride dispersant and the pure water of the dilution
Product is than being 1: 100-200.
Based on above-mentioned, in the step of mixing is stood, the volume of the hexagonal boron nitride micro mist and the pure water
Than for 1: 10-25.
Include based on above-mentioned, the step of the ultrasonic vibration：The pre-dispersed system of the hexagonal boron nitride is placed in ultrasonic wave
In cleaning machine, using frequency ＞ 20kHz ultrasonic oscillation 5-30 minutes, the hexagonal boron nitride stable dispersion system is obtained.
In the hexagonal boron nitride dispersant that the present invention is provided, the anion surfactant is soluble in water, table
Face tension force is small, with good dispersiveness, especially sodium alkyl benzene sulfonate or lauryl sodium sulfate；C16 unrighted acids
Available for the intermediate of various surfactants, mainly for the production of the original of soap, lubricant, softening agent and synthetic detergent
Material；Carboxymethyl cellulose（CMC）, its aqueous solution have water tariff collection, colloid protection, emulsification and suspend etc. effect；Nonyl phenol gathers
Oxygen vinethene for nonyl phenol and oxirane the condensation reaction under catalyst action nonionic surfactant, have it is various not
Same hydrophilic lipophilic balance, there is good infiltration, emulsification, scattered, hard water resistance, anti-reduction, oxidation resistance；Fatty acid ethanolamide
Acid amides belongs to nonionic surfactant, can be with a variety of surfactant compatibilities；Ethoxylation sodium sulfonate is relative to other anion
Surfactant, belongs to low froth pulp, and have good stability in hard water energy and low temperature flowability；N, N- are double（Polyoxyethylene）
The alkalescent of alkyl amine n-oxide makes it show nonionic nature in neutral and alkaline solution, in acid medium in sun from
Sub- property, is a kind of multi-functional amphoteric surfactant, can be used as the accelerator of anion surfactant；Sodium hydroxide can rise
To the effect of catalyst, occurs saponification：RCOOR'+ NaOH=RCOONa+R'OH, also for neutralizing aliphatic acid, are adjusted
Save pH value.
Therefore, each component in the hexagonal boron nitride dispersant that the present invention is provided cooperates, and cooperates, can cause
Hexagonal boron nitride powder equably, stably disperses, it is to avoid or reduce the possibility reunited；And the process for dispersing that the present invention is provided
Carry out in confined conditions, to prevent from standing and operating for a long time so that the pollutant such as dust is fallen into dispersion, shadow
Ring the accuracy of final testing result；So, the hexagonal boron nitride dispersant and process for dispersing provided using the present invention can be solved
Easily go out when certainly disperseing the scattered uneven of hexagonal boron nitride micro mist presence, detection granularity and distribution using silicate in the prior art
It is existing bimodal, and detection granularity, size distribution and true granularity, size distribution problem devious, while can also reduce to swashing
The damage of light Particle Size Analyzer sample room, makes the hexagonal boron nitride micro mist of the easy moisture absorption of reunion be more easy to disperse.
Brief description of the drawings
The particle size distribution figure of trickle powder in the hexagonal boron nitride dispersion that Fig. 1 provides for the embodiment of the present invention 1.
The particle size distribution figure of trickle powder in the hexagonal boron nitride dispersion that Fig. 2 provides for the embodiment of the present invention 2.
The particle size distribution figure of trickle powder in the hexagonal boron nitride dispersion that Fig. 3 provides for the embodiment of the present invention 3.
The particle size distribution figure of trickle powder in the hexagonal boron nitride dispersion that Fig. 4 provides for the embodiment of the present invention 4.
Embodiment
Below by embodiment, technical scheme is described in further detail.Wherein, it is each below
The granularity of the hexagonal boron nitride powder used in embodiment is measured using ESEM, the hexagonal boron nitride stable dispersion
The granularity of hexagonal boron nitride particles in system is measured using Malvern laser particle analyzer Mastersizer 2000.
Embodiment 1
The embodiment of the present invention 1 provides a kind of hexagonal boron nitride dispersant, and the formula of the dispersant is as shown in table 1：
The formula of the hexagonal boron nitride dispersant of table 1
| Component | Mass fraction（wt%） |
| Sodium alkyl benzene sulfonate | 9.0 |
| C16 unrighted acids | 5.0 |
| Carboxymethyl cellulose | 4.0 |
| NPE | 3.0 |
| Fatty acid ethanol amide | 3.0 |
| Ethoxylation sodium sulfonate | 2.0 |
| N, N- are double（Polyoxyethylene）Alkyl amine n-oxide | 1.0 |
| Sodium hydroxide | 1.0 |
| Pure water | 72.0 |
The present embodiment also provides a kind of process for dispersing of hexagonal boron nitride, comprises the following steps：It is 0-0.5 μm to take granularity
The g of hexagonal boron nitride micro mist 0.015 be placed in test tube, while add 0.5 ml dispersion liquid, then add pure water, and
The volume ratio of the hexagonal boron nitride micro mist and the pure water is about 1:10；Then test tube port is sealed with film, nature is sealed
Stand sample 48 hours；Ultrasonic oscillation 5 minutes, the frequency of ultrasonic wave is 40-50 kHz, constantly rocks test tube and shakes up sample i.e.
The hexagonal boron nitride stable dispersion system is can obtain, wherein, the dispersion liquid is six sides nitridation prepared by the formula shown in table 1
The dilute solution of borated dispersant, and in the dispersion liquid, above-mentioned hexagonal boron nitride dispersant and the pure water of the dilution
Volume ratio is 1: 100.As seen from Figure 1：Hexagonal boron nitride particles in the hexagonal boron nitride stable dispersion system
Granularity D5 is 0.139 μm, and D95 is 0.407 μm, with the granularity 0- for the hexagonal boron nitride micro mist not being dispersed in before the dispersion liquid
0.5 μm of comparison coincide.
Embodiment 2
The embodiment of the present invention 2 provides a kind of hexagonal boron nitride dispersant, and the formula of the dispersant is as shown in table 2：
The formula of the hexagonal boron nitride dispersant of table 2
| Component | Mass fraction（wt%） |
| Sodium alkyl benzene sulfonate | 10.0 |
| C16 unrighted acids | 4.0 |
| Carboxymethyl cellulose | 5.0 |
| NPE | 2.0 |
| Fatty acid ethanol amide 2.0-4.0 | 4.0 |
| Ethoxylation sodium sulfonate | 3.0 |
| N, N- are double（Polyoxyethylene）Alkyl amine n-oxide | 1.5 |
| Sodium hydroxide | 0.5 |
| Pure water | 70.0 |
The present embodiment also provides a kind of process for dispersing of hexagonal boron nitride, comprises the following steps：The granularity for taking 0.040 g is
0-1 μm of hexagonal boron nitride micro mist is placed in test tube, while adding 1 ml dispersion liquid, then adds pure water, and described
The volume ratio of hexagonal boron nitride micro mist and pure water is about 1:15；Then test tube port is sealed with plug, sealing nature stands sample
Product 48 hours；Ultrasonic oscillation 15 minutes, the frequency of ultrasonic wave is 40-45 kHz, and constantly rocking test tube and shaking up sample to obtain
To the hexagonal boron nitride stable dispersion system, wherein, six sides that the dispersion liquid is prepared as the formula shown in pure water and table 2
Borated dispersant composition is nitrogenized, and in the dispersion liquid, the body of above-mentioned hexagonal boron nitride dispersant and the pure water of the dilution
Product is than being 1: 150.As seen from Figure 2：The grain of hexagonal boron nitride particles in the hexagonal boron nitride stable dispersion system
It is 0.327 μm to spend D5, and D95 is 0.868 μm, with the granularity 0-1 for the hexagonal boron nitride micro mist not being dispersed in before the dispersion liquid
μm comparison coincide.
Embodiment 3
The embodiment of the present invention 3 provides a kind of hexagonal boron nitride dispersant, and the formula of the dispersant is as shown in table 3：
The formula of the hexagonal boron nitride dispersant of table 3
| Component | Mass fraction（wt%） |
| Lauryl sodium sulfate | 8.0 |
| C17 unrighted acids | 6.0 |
| Carboxymethyl cellulose | 3.0 |
| NPE | 2.0 |
| Fatty acid ethanol amide | 2.0 |
| Ethoxylation sodium sulfonate | 1.5 |
| N, N- are double（Polyoxyethylene）Alkyl amine n-oxide | 0.5 |
| Sodium hydroxide | 0.5 |
| Pure water | 76.5 |
The present embodiment also provides a kind of process for dispersing of hexagonal boron nitride, comprises the following steps：Take 0.060 g granularity about
It is placed in test tube, while adding 1.5 ml dispersion liquid, then adds appropriate for 0.5-1.5 μm of hexagonal boron nitride micro mist
Pure water, and the volume ratio of the hexagonal boron nitride micro mist and the pure water is about 1:20；Then test tube port is sealed with film,
Seal nature and stand sample 56 hours；Ultrasonic oscillation 20 minutes, the frequency of ultrasonic wave is 30-40 kHz, constantly rocks test tube
Shake up sample and can obtain the hexagonal boron nitride stable dispersion system, wherein, the dispersion liquid is as shown in pure water and table 3
Hexagonal boron nitride dispersant composition prepared by formula, and in the dispersion liquid, above-mentioned hexagonal boron nitride dispersant and the dilution
The volume ratio of pure water is 1: 130.As seen from Figure 3：Six sides in the hexagonal boron nitride stable dispersion system
The granularity D5 of boron nitride particle is 0.503 μm, and D95 is 1.306 μm, with the hexagonal boron nitride not being dispersed in before the dispersion liquid
0.5-1.5 μm of comparison of granularity of micro mist coincide.
Embodiment 4
The embodiment of the present invention 4 provides a kind of hexagonal boron nitride dispersant, and the formula of the dispersant is as shown in table 4：
The formula of the hexagonal boron nitride dispersant of table 4
| Component | Mass fraction（wt%） |
| Sodium alkyl benzene sulfonate and lauryl sodium sulfate | 10.0 |
| C18 unrighted acids | 4.5 |
| Carboxymethyl cellulose | 3.5 |
| NPE | 3.5 |
| Fatty acid ethanol amide | 2.6 |
| Ethoxylation sodium sulfonate | 1.7 |
| N, N- are double（Polyoxyethylene）Alkyl amine n-oxide | 0.5 |
| Sodium hydroxide | 1.5 |
| Pure water | 72.2 |
The present embodiment also provides a kind of process for dispersing of hexagonal boron nitride, comprises the following steps：Take 0.080 g granularity about
It is placed in for 1-3 μm of hexagonal boron nitride micro mist in test tube, while adding 2 ml dispersion liquid, then adds pure water, and institute
The volume ratio for stating hexagonal boron nitride micro mist and the pure water is about 1:25；Then test tube port is sealed with film, sealing nature is quiet
Put sample 72 hours；Ultrasonic oscillation 30 minutes, the frequency of ultrasonic wave is 20-30 kHz, constantly rocks test tube and shakes up sample i.e.
The hexagonal boron nitride stable dispersion system is can obtain, wherein, the dispersion liquid is prepared as the formula shown in pure water and table 4
Hexagonal boron nitride dispersant is constituted, and in the dispersion liquid, above-mentioned hexagonal boron nitride dispersant and the pure water of the dilution
Volume ratio be 1: 200.As seen from Figure 4：Hexagonal boron nitride particles in the hexagonal boron nitride stable dispersion system
Granularity D5 be 1.003 μm, D95 is 2.882 μm, with the granularity for the hexagonal boron nitride micro mist not being dispersed in before the dispersion liquid
1-3 μm of comparison coincide.
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, those of ordinary skills in the art should understand that：Still
The embodiment of the present invention can be modified or equivalent substitution is carried out to some technical characteristics；Without departing from this hair
The spirit of bright technical scheme, it all should cover among claimed technical scheme scope of the invention.
Claims (7)
1. a kind of hexagonal boron nitride dispersant, it is characterised in that it includes the component of following mass percent：Alkyl anion table
Face activating agent 8.0%-10.0%, C16-18 unrighted acid 4.0%-6.0%, carboxymethyl cellulose 3.0%-5.0%, nonyl phenol gather
Oxygen vinethene 2.0%-4.0%, fatty acid ethanol amide 2.0-4.0%, ethoxylation sodium sulfonate 1.0%-3.0%, N, N- is double（Polyoxy
Ethene）Alkyl amine n-oxide 0.5%-1.5%, sodium hydroxide 0.5%-1.5%, remaining is pure water.
2. the process for dispersing of hexagonal boron nitride according to claim 1, it is characterised in that live on the alkyl anion surface
Property agent be sodium alkyl benzene sulfonate, lauryl sodium sulfate or its any combination.
3. a kind of process for dispersing of hexagonal boron nitride, it comprises the following steps：
Mixing is stood：0.015-0.080 g hexagonal boron nitrides micro mist, 0.5-2 ml dispersion liquid and pure water are mixed, and it is close
Envelope stands 36-72 hours, obtains the pre-dispersed system of hexagonal boron nitride, wherein, the dispersion liquid is as described in claim 1 or 2
Hexagonal boron nitride dispersant and the pure water of dilution composition；
Ultrasonic vibration：Using the pre-dispersed system of hexagonal boron nitride described in ultrasonic oscillation, hexagonal boron nitride stabilising dispersions are obtained
System.
4. the process for dispersing of hexagonal boron nitride according to claim 3, it is characterised in that described in the dispersion liquid
The volume ratio of hexagonal boron nitride dispersant and the pure water of the dilution is 1: 100-200.
5. the process for dispersing of the hexagonal boron nitride according to claim 3 or 4, it is characterised in that stood in the mixing
In step, the volume ratio of the hexagonal boron nitride micro mist and the pure water is 1: 10-25.
6. the process for dispersing of hexagonal boron nitride according to claim 5, it is characterised in that wrap the step of the ultrasonic vibration
Include：The pre-dispersed system of the hexagonal boron nitride is placed in supersonic wave cleaning machine, using frequency ＞ 20kHz ultrasonic oscillation 5-
30 minutes, obtain the hexagonal boron nitride stable dispersion system.
7. the process for dispersing of hexagonal boron nitride according to claim 3, it is characterised in that wrap the step of the ultrasonic vibration
Include：The pre-dispersed system of the hexagonal boron nitride is placed in supersonic wave cleaning machine, using frequency ＞ 20kHz ultrasonic oscillation 5-
30 minutes, obtain the hexagonal boron nitride stable dispersion system.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4195002A (en) * | 1978-07-27 | 1980-03-25 | International Lead Zinc Research Organization, Inc. | Water-dispersible coatings containing boron nitride for steel casting dies |
| CN1269273A (en) * | 1999-04-07 | 2000-10-11 | 桑德维克公司 | Materials based on porous cubic crystal series boron nitride for post production of cutting tools and preparation method thereof |
| CN1538908A (en) * | 2001-08-07 | 2004-10-20 | ʥ�걾�մɼ����Ϲɷ�����˾ | High solid HBV slurry, paste, spherical powder, and method of making and using them |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4195002A (en) * | 1978-07-27 | 1980-03-25 | International Lead Zinc Research Organization, Inc. | Water-dispersible coatings containing boron nitride for steel casting dies |
| CN1269273A (en) * | 1999-04-07 | 2000-10-11 | 桑德维克公司 | Materials based on porous cubic crystal series boron nitride for post production of cutting tools and preparation method thereof |
| CN1538908A (en) * | 2001-08-07 | 2004-10-20 | ʥ�걾�մɼ����Ϲɷ�����˾ | High solid HBV slurry, paste, spherical powder, and method of making and using them |
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