CN106400486B - A kind of surface modifying method of magnesium borate crystal whisker - Google Patents
A kind of surface modifying method of magnesium borate crystal whisker Download PDFInfo
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- CN106400486B CN106400486B CN201610762130.8A CN201610762130A CN106400486B CN 106400486 B CN106400486 B CN 106400486B CN 201610762130 A CN201610762130 A CN 201610762130A CN 106400486 B CN106400486 B CN 106400486B
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- plasma
- crystal whisker
- borate crystal
- magnesium borate
- plasma apparatus
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Abstract
The invention discloses a kind of surface modifying method of magnesium borate crystal whisker, comprising steps of A, magnesium borate crystal whisker is placed in plasma apparatus, and vacuumized；B, non-polymerization gas is passed through in plasma apparatus, plasma apparatus is adjusted to the first air pressure and the first discharge power, so that non-polymerization gas is discharged under electric field action and generate the first plasma, the surface of the surface action of the first plasma and magnesium borate crystal whisker, magnesium borate crystal whisker generates active group；C, stop introducing non-polymerization gas, polymerizable monomer is introduced into plasma apparatus simultaneously, plasma apparatus is adjusted to the second air pressure and the second discharge power, so that polymerizable monomer is discharged under electric field action and generates the second plasma, second plasma is reacted with active group, obtains boric acid modification magnesium whisker.The surface modifying method of magnesium borate crystal whisker according to the present invention coats organic coating film by chemical bond on the surface of magnesium borate crystal whisker, and structure is more stable；Meanwhile the surface is modified time-consuming shorter.
Description
Technical field
The invention belongs to process for modifying surface fields, it relates in particular to which a kind of surface of quick magnesium borate crystal whisker changes
Property method.
Background technique
Magnesium borate crystal whisker also known as pyroboric acid magnesium whisker, molecular formula Mg2B2O5.Magnesium borate crystal whisker is because having excellent power
The advantages that learning performance, heat resistance, corrosion resistance, and be widely used in almag and high molecular material.Work as antifungin
When whisker is doped in other materials, not only show good enhancing performance when enhancing composite material, and have lightweight,
High-ductility, it is wear-resisting, corrosion-resistant the features such as.
But magnesium borate crystal whisker is as a kind of inorganic compound, with very strong hydrophily and biggish specific surface
Product, when it is in conjunction with hydrophobic macromolecule matrix, has the problem of poor compatibility, causes magnesium borate crystal whisker in the macromolecule
Disperse unevenness in matrix, interface binding power is poor, and it is undesirable that this will result directly in application effect.It therefore, is raising magnesium borate crystal whisker
The binding force between dispersibility and interface in macromolecule matrix, it is necessary to which table is carried out to magnesium borate crystal whisker using specific technique
Face is modified.
Magnesium borate crystal whisker is modified generally using borate as coupling agent at present.Borate is a kind of
Center and the substance with boron-oxygen skeleton, borate can generate good physisorption between magnesium borate crystal whisker,
So as to improve the compatibility between magnesium borate crystal whisker and macromolecule matrix.But when borate is as coupling agent, rely primarily on point
Active force is combined with magnesium borate crystal whisker surface between son, and the physical absorption binding force due to caused by intermolecular force is more chemical
Key is weak, and heat of adsorption is smaller, and absorption and desorption rate easily cause modified magnesium borate crystal whisker to change in external environment also all than very fast
Chronotropismus can be unstable.In addition, after being modified as coupling agent to magnesium borate crystal whisker using borate, it is also necessary to rear place
Reason, time-consuming, and technique is also relative complex.
Summary of the invention
To solve the above-mentioned problems of the prior art, the present invention provides a kind of using plasma activation-grafting
Square technology carries out the surface modifying method of magnesium borate crystal whisker, which makes magnesium borate crystal whisker surface coat one layer
Organic coating film, to achieve the purpose that be modified the surface of magnesium borate crystal whisker；And the surface modifying method is by chemistry
Bond is closed, stable structure, and modification time is short.Plasma-activated-crosslinking technology be first with non-polymerization gas generate it is equal from
The surface action of son and magnesium borate crystal whisker makes the surface of magnesium borate crystal whisker generate active group, then passes to polymerism gas,
It generates free radicals under discharge condition, and is reacted with the active group on the surface of magnesium borate crystal whisker, be grafted to the table of magnesium borate crystal whisker
Face.One layer of organic coating film is formed on the surface of magnesium borate crystal whisker, to achieve the purpose that surface is modified.
In order to achieve the above object of the invention, present invention employs the following technical solutions:
A kind of surface modifying method of magnesium borate crystal whisker, comprising steps of A, magnesium borate crystal whisker is placed in plasma apparatus,
And the plasma apparatus is vacuumized；B, non-polymerization gas is introduced into the plasma apparatus, is adjusted described etc.
Ion device makes the non-polymerization gas discharge under electric field action and generates first etc. to the first air pressure and the first discharge power
Gas ions, first plasma are reacted with the surface of the magnesium borate crystal whisker, and the surface of the magnesium borate crystal whisker generates work
Property group；C, stop introducing the non-polymerization gas, while polymerizable monomer being introduced into the plasma apparatus, adjust institute
Plasma apparatus is stated to the second air pressure and the second discharge power, so that the polymerizable monomer is discharged under electric field action and generates second
Plasma, second plasma are reacted with the active group, obtain boric acid modification magnesium whisker.
Further, in the step A, it is 5Pa~10Pa that the plasma apparatus, which is evacuated to its vacuum degree,.
Further, in the step B, the non-polymerization gas is passed through into the plasma apparatus, until
The pressure of the plasma apparatus is 40Pa~90Pa.
Further, in the step B, the non-polymerization gas is selected from Ar, O2In any one.
Further, in the step B, first discharge power is 50W~100W.
Further, in the step B, the discharge time of the plasma apparatus is 2min~5min.
Further, in the step C, the polymerizable monomer is passed through in the plasma apparatus, until described
The pressure of plasma apparatus is 20Pa~70Pa.
Further, in the step C, the polymerizable monomer is selected from styrene, acrylic acid, methymethacrylate
With any one in hexamethylene.
Further, in the step C, second discharge power is 30W~80W.
Further, in the step C, the discharge time of the plasma apparatus is 2min~10min.
The present invention is by the ionization to non-polymerization gas and polymerizable monomer respectively twice, so that magnesium borate crystal whisker is completed
The modified process in the surface of plasma-activated-grafting.Specifically, first by being ionized simultaneously to non-polymerization gas
It is reacted with magnesium borate crystal whisker, which is activated, so that its surface forms active group；Then by polymerism
Monomer carry out ionize and react with the above-mentioned magnesium borate crystal whisker through overactivation, polymerizable monomer through ionization generate plasma and
Active group reaction forms one layer of organic coating film on the surface of magnesium borate crystal whisker, to obtain boric acid modification magnesium whisker.It compares
It is modified in the surface of the surface modifying method in the prior art using borate as coupling agent, magnesium borate crystal whisker of the invention
Method can be by chemical bonds surface-modifying groups (the organic coating film i.e. in the present invention) and magnesium borate crystal whisker, and structure is more
Add stabilization；Meanwhile the process that the surface is modified is simple, time-consuming shorter.
Detailed description of the invention
What is carried out in conjunction with the accompanying drawings is described below, above and other aspect, features and advantages of the embodiment of the present invention
It will become clearer, in attached drawing:
Fig. 1 is the structural schematic diagram of the plasma apparatus of embodiment according to the present invention.
Specific embodiment
Hereinafter, will be described in the embodiment of the present invention.However, it is possible to implement the present invention in many different forms,
And the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, provide these embodiments be in order to
The principle of the present invention and its practical application are explained, to make others skilled in the art it will be appreciated that various realities of the invention
Apply example and the various modifications for being suitable for specific intended application.
Term " first ", " second " etc. herein can be used to describe various substances although will be appreciated that, these
Substance should not be limited by these terms.These terms are only used to distinguish a substance with another substance.
The invention discloses a kind of surface modifying methods of magnesium borate crystal whisker, specifically comprise the following steps:
Step 1: the preparation of equipment.
Specifically, magnesium borate crystal whisker is placed in plasma apparatus, the plasma apparatus is as shown in Figure 1.
The plasma apparatus includes a reaction chamber for reaction, reactant (the non-polymerization gas in such as the application
Body and polymerizable monomer) it can be introduced inside the reaction chamber by a pipeline；Meanwhile the reaction chamber is also connected with vacuum
Pump, to control the pressure inside reaction chamber.Each operation of above-mentioned progress is in a motor being connected on reaction chamber
Cooperation under complete.
The plasma apparatus is vacuumized；Specifically, by the plasma apparatus be evacuated to its vacuum degree be 5Pa~
10Pa。
Step 2: the preparation of active magnesium borate crystal whisker.
Specifically, non-polymerization gas is passed through in the plasma apparatus to its internal pressure is 40Pa~90Pa；
Plasma apparatus is adjusted to the discharge power of 50W~100W again, which discharges and generate under electric field action
First plasma, the first plasma is reacted with magnesium borate crystal whisker so that the surface of magnesium borate crystal whisker generates active group.
Preferably, the non-polymerization gas is selected from Ar, O2In any one；And the discharge time of the plasma apparatus
For 2min~5min.In this way, obtaining active magnesium borate crystal whisker.
Step 3: the acquisition of boric acid modification magnesium whisker.
Specifically, after to magnesium borate crystal whisker activation, stopping is passed through the non-polymerization gas, while by polymerism
It is 20Pa~70Pa that monomer, which is passed through in the plasma apparatus to its internal pressure,；Again by plasma apparatus be adjusted to 30W~
The discharge power of 80W, the polymerizable monomer discharge under electric field action generate the second plasma, the second plasma with it is described
Active group reaction, obtains boric acid modification magnesium whisker.
Preferably, the polymerizable monomer is any in styrene, acrylic acid, methymethacrylate and hexamethylene
It is a kind of；And the discharge time of the plasma apparatus is 2min~10min.In this way, passing through chemistry on the surface of magnesium borate crystal whisker
The form of key coats an organic coating film, to complete modified to the surface of magnesium borate crystal whisker.
The activation index and contact angle of the boric acid modification magnesium whisker of acquisition are tested.
Above-mentioned preparation method of the invention will be embodied by specific embodiment below；In order to compare in each embodiment not
Same condition lists the conditional parameter of embodiment 1-4 in table form and is modified result.
The conditional parameter of 1 embodiment 1-4 of table and modified Comparative result
As it can be seen from table 1 the surface modifying method modification degree of the magnesium borate crystal whisker of embodiment according to the present invention is high,
The magnesium borate crystal whisker hydrophobic performance of acquisition is good, and overall modified effect is good, meanwhile, method of modifying is simple, and time-consuming shorter, and one
As can be completed in 4min~15min；In addition, the surface modifying method is in a manner of forming chemical bond in magnesium borate crystal whisker
The organic coating film formed on surface, thus compared with the prior art in some method of modifying structures it is more firm.
Although the present invention has shown and described referring to specific embodiment, it should be appreciated by those skilled in the art that:
In the case where not departing from the spirit and scope of the present invention being defined by the claims and their equivalents, can carry out herein form and
Various change in details.
Claims (10)
1. a kind of surface modifying method of magnesium borate crystal whisker, which is characterized in that comprising steps of
A, magnesium borate crystal whisker is placed in plasma apparatus, and the plasma apparatus is vacuumized；
B, non-polymerization gas is introduced into the plasma apparatus, adjusts the plasma apparatus to the first air pressure and first and puts
Electrical power, make the non-polymerization gas discharge under electric field action generate the first plasma, first plasma with
The surface of the surface action of the magnesium borate crystal whisker, the magnesium borate crystal whisker generates active group；
C, stop introducing the non-polymerization gas, while polymerizable monomer being introduced into the plasma apparatus, described in adjusting
Plasma apparatus makes the polymerizable monomer discharge under electric field action and generates second etc. to the second air pressure and the second discharge power
Gas ions, second plasma are reacted with the active group, obtain boric acid modification magnesium whisker.
2. surface modifying method according to claim 1, which is characterized in that in the step A, the plasma is set
Standby its vacuum degree that is evacuated to is 5Pa~10Pa.
3. the method according to claim 1, wherein in the step B, first air pressure be 40Pa~
90Pa。
4. surface modifying method according to claim 1, which is characterized in that in the step B, the non-polymerization gas
Body is selected from Ar, O2In any one.
5. the method according to claim 1, wherein first discharge power is 50W in the step B
~100W.
6. surface modifying method according to claim 1, which is characterized in that in the step B, the plasma apparatus
Discharge time be 2min~5min.
7. the method according to claim 1, wherein in the step C, second air pressure be 20Pa~
70Pa。
8. surface modifying method according to claim 1, which is characterized in that in the step C, the polymerizable monomer
Any one in styrene, acrylic acid, methymethacrylate and hexamethylene.
9. surface modifying method according to claim 1, which is characterized in that in the step C, the second electric discharge function
Rate is 30W~80W.
10. surface modifying method according to claim 1, which is characterized in that in the step C, the plasma is set
Standby discharge time is 2min~10min.
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| CN108642957A (en) * | 2018-06-01 | 2018-10-12 | 合肥语林装饰工程有限公司 | A kind of wallpaper PVC paste material |
| CN108797199A (en) * | 2018-06-01 | 2018-11-13 | 合肥语林装饰工程有限公司 | A kind of preparation method with excellent electro-magnetic wave absorption wallpaper thickener |
| CN108660853A (en) * | 2018-06-01 | 2018-10-16 | 合肥月煌新型装饰材料有限公司 | A kind of PVC foam Wallpaper paste material composition |
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| CN101701079A (en) * | 2009-10-30 | 2010-05-05 | 昆明春叶塑料制成品有限公司 | Preparation method of polyethylene mulching film master batch for magnesium salt whisker reinforced smoke |
| CN101705458A (en) * | 2009-11-11 | 2010-05-12 | 青海大学 | Preparation process of modified magnesium borate crystal whisker reinforced magnesium-matrix composite material |
| CN101709509A (en) * | 2009-12-10 | 2010-05-19 | 太原理工大学 | Method for preparing magnesium borate whisker |
| CN102321395A (en) * | 2011-08-30 | 2012-01-18 | 成都理工大学 | Method for surface modification of magnesium borate crystal whisker by using borate coupling agent |
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- 2016-08-30 CN CN201610762130.8A patent/CN106400486B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701079A (en) * | 2009-10-30 | 2010-05-05 | 昆明春叶塑料制成品有限公司 | Preparation method of polyethylene mulching film master batch for magnesium salt whisker reinforced smoke |
| CN101705458A (en) * | 2009-11-11 | 2010-05-12 | 青海大学 | Preparation process of modified magnesium borate crystal whisker reinforced magnesium-matrix composite material |
| CN101709509A (en) * | 2009-12-10 | 2010-05-19 | 太原理工大学 | Method for preparing magnesium borate whisker |
| CN102321395A (en) * | 2011-08-30 | 2012-01-18 | 成都理工大学 | Method for surface modification of magnesium borate crystal whisker by using borate coupling agent |
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