CN106141164A - A kind of preparation method of nm-class Ti polymer - Google Patents
A kind of preparation method of nm-class Ti polymer Download PDFInfo
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- CN106141164A CN106141164A CN201510193930.8A CN201510193930A CN106141164A CN 106141164 A CN106141164 A CN 106141164A CN 201510193930 A CN201510193930 A CN 201510193930A CN 106141164 A CN106141164 A CN 106141164A
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- rotating cylinder
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Abstract
The invention provides the preparation method of a kind of nm-class Ti polymer; it will in titanium valve 100, help disintegrator 0.5～30, protective agent 0.1～20, dispersant 100～1000 ratio to be mixed into mixture system; on homemade high-energy and high-efficiency pulverizer; by pulverizing; complete mechanico-chemical reaction, thus obtain nm-class Ti polymer.Additionally provide self-control high-energy and high-efficiency crushing machine device (see photo).It provides possibility for nm-class Ti polymer paint preparation, provides possibility for weld seam coating material production, energy-conservation antiscale coating material production, the production of titanium healant.It is a kind of active filler, is again a kind of coupling agent, has special effect in terms of the corrosion resistance providing coating and antiscale.
Description
Technical field
The present invention designs the preparation method of a kind of nm-class Ti polymer, belongs to the manufacture field of nanotechnology metal powder, the invention still further relates to this preparation side
Self-control high-energy and high-efficiency pulverizer used by method.
Background technology
Along with the progress of science and technology, people are more and more higher to the performance requirement of polymeric material, use modified filler that polymeric material can be made to have some
Special performance, such as electric conductivity, magnetic conductivity, heat conductivity, corrosion resistance, suction ripple, extinction etc., therefore research new packing is current most active section
Grind one of problem.Along with the appearance of nano material, study the novel nano-material modification Environment Science problem especially to polymeric material.
As industrial corrosion-resistant basic material, titanium is only second to tantalum, niobium, but its price is relatively low.It is that people are chased after always that titanium is made titanium
Ask.
Summary of the invention
The purpose of the present invention is to provide the preparation method of a kind of nm-class Ti polymer just, can be obtained for modification by this easy manufacture method
Filler needed for polymeric material, such that it is able to be modified multiple polymers, it is thus achieved that has the macromolecular material of novel performance.
The object of the present invention is achieved like this, and metallic titanium powder is mixed into mixture system with helping disintegrator, protective agent with certain proportion by it, utilizes
Homemade high-energy and high-efficiency pulverizer, by pulverizing, completes mechanico-chemical reaction, thus obtains nm-class Ti polymer.
Further object is that a kind of high-energy and high-efficiency pulverizer implementing said method of offer, this pulverizer includes the main shaft C being parallel to each other
Being driven rotation with countershaft F, main shaft C by motor A, countershaft F is driven or by independent system by the speed change gear B by main shaft C transmission
Directly driving, at least two rotating cylinder D rotate around countershaft F, are driven operating by main shaft C simultaneously, and wherein the speed of mainshaft is set as 100-1000rpm,
The rotating ratio of main shaft C and countershaft F is set as 1: 2-10, and the draw ratio of rotating cylinder D is at least 10: 1.
The core technology content of the preparation method of the nm-class Ti polymer described in the present invention is that nm-class Ti polymer (by weight) is prepared formula and is:
Wherein:
The described disintegrator that helps is to have oligomer or the polymer of unsaturated functional group, including polyvinyl acetate, polypropylene acid esters, low-molecular-weight
In polyamide, oleic acid, polysiloxanes one or more；Described protective agent is pf resin of low molecular weight and prepolymer, epoxide, Korea Spro
Sulphur rubber, chlorinated rubber, polyvinyl alcohol, poly-aluminum ethylsiloxane, polysiloxanes one or more；
Described dispersant is one or more in aromatic series, styrene, hydro carbons, chlorocarbon class, alcohols, ketone acetates；
To be furnished with the above-mentioned titanium valve helping disintegrator, protective agent and dispersant, install in the pulverizer of high-energy and high-efficiency, through pulverizing, produce fineness
The ultra-fine nm-class Ti polymer of black of 10-100nm.
Accompanying drawing explanation
Fig. 1 is the high-energy and high-efficiency pulverizer schematic diagram described in the present invention.
Detailed description of the invention
The present invention is further described, it is clear that these particular contents are not the restriction of scope below in conjunction with concrete example.Wherein
Described particle diameter uses electron microscopy to measure, and specific surface area uses cryogenic gas determination of adsorption method.
Embodiment 1
It is 1: 1-1.6 wiring solution-forming by phenol and formaldehyde by mole ratio, under sodium hydroxide effect, is stirred at reflux 20-30min, through dehydration, obtains
Obtain the protectant prepolymer of phenolic resin of certain viscosity.
Take above-mentioned phenolic resin prepolymer 200g, add dispersant ethanol 800g, help disintegrator oleic acid 80g, react 1.5h at 50-60 DEG C, filter
Obtain light brown gummy liquid.
Taking titanium valve 100g, add aforesaid liquid 70g, dispersant ethanol 630g, room temperature places 24h, charging, utilizes high-energy and high-efficiency pulverizer to pulverize
3.5h, it is thus achieved that specific surface area is 8.8m2The nm-class Ti polymer of/g.
Embodiment 2
By bisphenol-A 22.5mol, epoxychloropropane 225mol, water 104g, put in reactor, under cooling, stirring, be gradually added into 18g hydrogen-oxygen
Changing sodium, after 90-100 DEG C of condensation completes, add benzene desalination and reclaim low molecular weight epoxy compound, its molecular weight is 100-170.
Take this epoxide 100g (protective agent), add dispersant toluene 500g, help disintegrator polymethyl acrylate 10g, react 1.5h at 50 DEG C,
Reaction ends and puts into dispersant dimethylbenzene 200g, filters standby.
Take above-mentioned solution 100g, add titanium valve 100g, impregnate 24h, add dispersant toluene 800g mixing, powder on high-energy and high-efficiency pulverizer
Broken 4.5h, it is thus achieved that specific surface area is 10.5m2The nm-class Ti polymer of/g.
Embodiment 3
The polysiloxanes that the first polymers of disintegrator methyl methacrylate, 20g protective agent molecular weight are 800-1200 is helped to be gathered with 7g 100g titanium valve
Thing mixes, and at 70-80 DEG C of pretreatment 1h, adds dispersant pentanone 900g, be sufficiently mixed after cooling, and precipitation places 12h, adds dispersant fourth
Alcohol 100g, then pulverizes 1.5h on pulverizer, and using cryogenic gas absorption method to measure specific surface area is 5.8m2/g。
Embodiment 4
By 100g titanium valve first with dispersant ethyl acetate 400g impregnate 3h, be subsequently adding protective agent molecular weight be 1200-1800 containing sulphur rubber 8g,
Add and help disintegrator polyvinyl acetate 5g, be sufficiently mixed, then add 100g acetone, capryl alcohol 100g, utilize pulverizer to pulverize 5h, prepared titanium
Specific surface area 9.6m of nanometer polymer2/g。
Embodiment 5
The polyamide 20g helping disintegrator molecular weight to be 500-800 and protective agent low-viscosity chlorinated rubber 30g is added hot mixing, adds an innings siloxanes
5g, high-speed stirred 1h, it is subsequently added dispersant toluene: dimethylbenzene=50: the mixed liquid 500g of 50.
Take industry titanium valve 100g, add above-mentioned prepolymer 100g, add dimethylbenzene 500g, pulverizer is pulverized 2h, it is thus achieved that specific surface area is
10m2The nm-class Ti polymer of/g.
The invention still further relates to a kind of high-energy and high-efficiency pulverizer, particularly relate to realize the super-refinement of hard material, prepared by surface modification and metal-containing polymer,
The high-energy and high-efficiency pulverizer that nano material produces.
As shown in Figure 1, the high-energy and high-efficiency pulverizer described in the present invention includes main shaft C and the countershaft F being parallel to each other, and main shaft C is driven by motor A
Rotating, countershaft F is driven by the speed change gear B by main shaft C transmission or is directly driven by independent system, at least two rotating cylinder D around
Countershaft F rotates, and is driven operating by main shaft C simultaneously, and wherein the speed of mainshaft is set as 100-1000rpm, and the rotating ratio of main shaft C and countershaft F sets
Being 1: 2-10, the draw ratio of rotating cylinder D is at least 10: 1.
The originality of the pulverizer of the present invention be material is used crushing, grind, free impact comminution, impact comminution of being obstructed, split broken, roll over broken,
Shredding etc. and to integrate, at short notice, disposably material being crushed to less than 1 micron until being less than 100nm from macroscopic particles, it is not necessary to point
Level processes, and provides possibility for large-scale production nano material.
The structure of the high-energy and high-efficiency pulverizer of the present invention is described in detail below in conjunction with accompanying drawing.
Main shaft C welds two or more parallel revolving body E, rotating cylinder D is arranged between revolving body through countershaft F.Main shaft C is by motor
A drives rotation, and main shaft C rotates and drives countershaft F to drive rotating cylinder D operating through speed change gear B.Wherein the speed of mainshaft is set as 100-1000rpm,
The rotating ratio of main shaft C and countershaft F is set as between 1: 2-10.
The installation of rotating cylinder D is achieved in that rotating cylinder D two ends are connected with the support countershaft F at its two ends by flange, or rotating cylinder D itself
Play the effect of countershaft F simultaneously.
The draw ratio of rotating cylinder D is at least 10: 1.Be preferably 10: 1-30: 1, such as, as a diameter of 35mm, the length of rotating cylinder can reach 500mm,
And as a diameter of 89mm, its length is up to 2000mm.So can ensure that titanium valve be constantly in rotating cylinder thin layer state impacted, squeezed
Press, be grated, crushing effect is provided significantly.Wherein the drive manner of rotating cylinder D can lean on speed change gear B to drive support shaft F to rotate and drive and turn
Cylinder D rotates.A kind of drive manner of rotating cylinder D can lean on independent dynamical system, directly drives support shaft F to rotate, the independence of each rotating cylinder D
The rotation of rotation system to synchronize, in the same direction, same to rotating speed.
Can install on rotating cylinder according to actual needs finned fin or whole device install heat sink, the extension device life-span, the most favorably
In crush efficiency.
Claims (6)
1. the preparation method of nm-class Ti polymer, it is characterised in that formula is in parts by weight
Wherein:
The described disintegrator that helps is to have oligomer or the polymer of unsaturated functional group, including polyvinyl acetate
In ester, polypropylene acid esters, low molecular polyamides, oleic acid, polysiloxanes one or more；Described guarantor
Protect agent to be pf resin of low molecular weight and prepolymer, epoxide, Korea Spro's sulphur rubber, chlorinated rubber, gather
Vinyl alcohol, poly-aluminum ethylsiloxane, polysiloxanes one or more；
Described dispersant is in aromatic series, styrene, hydro carbons, chlorocarbon class, alcohols, ketone acetates one
Plant or multiple；
To be furnished with the above-mentioned titanium valve helping disintegrator, protective agent and dispersant, install in the pulverizer of high-energy and high-efficiency,
Through pulverizing, produce the ultra-fine nm-class Ti polymer of black of fineness 10-100nm.
2. self-control is exclusively used in the high-energy and high-efficiency pulverizer implemented described in claim 1, it is characterised in that this pulverizer bag
Including the main shaft C and countershaft F being parallel to each other, main shaft C is driven by motor A and rotates, and countershaft F is by by main shaft C
The speed change gear B of transmission is driven or is directly driven by independent system, at least two rotating cylinder D around
Countershaft F rotates, and is driven operating by main shaft C simultaneously, and wherein the speed of mainshaft is set as 100-1000rpm, main shaft
The rotating ratio of C and countershaft F is set as 1: 2-10, and the draw ratio of rotating cylinder D is at least 10: 1.
3., such as the pulverizer of right 2, wherein the installation of rotating cylinder D is achieved in that rotating cylinder D two ends are by method
Orchid is connected with the support countershaft F at its two ends, or rotating cylinder D itself plays the effect of countershaft F simultaneously.
4., such as the pulverizer of Claims 2 or 3, wherein the drive manner of rotating cylinder D can lean on speed change gear B to drive
Support shaft F rotates and drives rotating cylinder D to rotate.
5., such as the pulverizer of Claims 2 or 3, wherein the drive manner of rotating cylinder D can lean on independent dynamical system,
Directly driving support shaft F to rotate, the rotation of the independent rotation system of each rotating cylinder D to synchronize, in the same direction, together
Rotating speed.
6., such as the pulverizer of right 2, finned fin is wherein installed on rotating cylinder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510193930.8A CN106141164A (en) | 2015-04-22 | 2015-04-22 | A kind of preparation method of nm-class Ti polymer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510193930.8A CN106141164A (en) | 2015-04-22 | 2015-04-22 | A kind of preparation method of nm-class Ti polymer |
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| CN106141164A true CN106141164A (en) | 2016-11-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510193930.8A Pending CN106141164A (en) | 2015-04-22 | 2015-04-22 | A kind of preparation method of nm-class Ti polymer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111410898A (en) * | 2020-04-21 | 2020-07-14 | 哈尔滨鑫科纳米科技发展有限公司 | Rare metal heat-dissipation anticorrosive paint for L ED heat-dissipation fins and preparation method thereof |
| CN113198707A (en) * | 2021-05-13 | 2021-08-03 | 云南云天化红磷化工有限公司 | Method for repairing surface of flow passage component of phosphogypsum slurry pump |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5174512A (en) * | 1988-12-16 | 1992-12-29 | Snamprogetti S.P.A. | Grinding process and a continuous high-capacity micronizing mill for its implementation |
| CN1266760A (en) * | 2000-04-17 | 2000-09-20 | 薛峻峰 | Process for preparing nm-class Ti-base metal powder and its special grinding apparatus |
| CN1689731A (en) * | 2004-04-23 | 2005-11-02 | 许德成 | Preparation method of rare metal alloy nanometer powder |
| CN200948431Y (en) * | 2006-09-14 | 2007-09-19 | 关文达 | Grinding type disintegrator |
| CN201701968U (en) * | 2010-06-12 | 2011-01-12 | 任项杰 | Sugar cube crusher |
-
2015
- 2015-04-22 CN CN201510193930.8A patent/CN106141164A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5174512A (en) * | 1988-12-16 | 1992-12-29 | Snamprogetti S.P.A. | Grinding process and a continuous high-capacity micronizing mill for its implementation |
| CN1266760A (en) * | 2000-04-17 | 2000-09-20 | 薛峻峰 | Process for preparing nm-class Ti-base metal powder and its special grinding apparatus |
| CN1689731A (en) * | 2004-04-23 | 2005-11-02 | 许德成 | Preparation method of rare metal alloy nanometer powder |
| CN200948431Y (en) * | 2006-09-14 | 2007-09-19 | 关文达 | Grinding type disintegrator |
| CN201701968U (en) * | 2010-06-12 | 2011-01-12 | 任项杰 | Sugar cube crusher |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111410898A (en) * | 2020-04-21 | 2020-07-14 | 哈尔滨鑫科纳米科技发展有限公司 | Rare metal heat-dissipation anticorrosive paint for L ED heat-dissipation fins and preparation method thereof |
| CN113198707A (en) * | 2021-05-13 | 2021-08-03 | 云南云天化红磷化工有限公司 | Method for repairing surface of flow passage component of phosphogypsum slurry pump |
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Application publication date: 20161123 |