CN109261295A - A kind of solid phase synthesis ball grinder - Google Patents

A kind of solid phase synthesis ball grinder Download PDF

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Publication number
CN109261295A
CN109261295A CN201811040482.8A CN201811040482A CN109261295A CN 109261295 A CN109261295 A CN 109261295A CN 201811040482 A CN201811040482 A CN 201811040482A CN 109261295 A CN109261295 A CN 109261295A
Authority
CN
China
Prior art keywords
cover
filter membrane
valve
valve body
ball
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811040482.8A
Other languages
Chinese (zh)
Inventor
李平
张熙曼
孙风程
陈红余
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong First Medical University and Shandong Academy of Medical Sciences
Original Assignee
Taishan Medical University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Taishan Medical University filed Critical Taishan Medical University
Priority to CN201811040482.8A priority Critical patent/CN109261295A/en
Publication of CN109261295A publication Critical patent/CN109261295A/en
Pending legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18Details
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18Details
    • B02C17/1805Monitoring devices for tumbling mills

Abstract

The invention discloses a kind of solid phase synthesis ball grinders, which is characterized in that tank body, cover, vent valve and pressure gauge;Vent valve includes valve deck, spring, ball sealer, valve body, upper filter membrane clip, filter membrane, lower filter membrane clip and conical baffled;Vent valve is installed on the groove slot with sieve pore of cover, is screwed by fixator;The pressure gauge is installed in the pressure gauge mounting hole on cover, is threadedly coupled.The present invention is realized using sealing ball-milling device to the controlled release for generating gas is chemically reacted during solid-phase ball milling, and structure is simple, convenient for safeguarding, easily operated.

Description

A kind of solid phase synthesis ball grinder
Technical field
The present invention relates to grinding ball grinding jars, in particular for the ball grinder of solid phase synthesis.
Background technique
Solid state reaction is very important one kind in chemical industry.Such synthetic reaction is mainly used in Gao Rong in early days Point insoluble solid, such as the pyroreaction system between silicate, oxide, solid alloy.Relative to solution chemical system, this Class synthesis technology has the characteristics that high temperature, highly energy-consuming, chemical reaction rate are slow, and people are always confined to explore in various solution each The new technique for synthesizing of substance.In recent years, it chemically reacts and studies about rare earth, so that solid state reaction is especially organic The unique advantage of synthesis in solid state is gradually excavated and is recognized.
Solid phase reaction is " surface reaction ", the especially reaction between solid-phase reactant, solid particle size, surface reaction Property has vital influence for reaction.It is synthesized especially for middle Low Temperature Solid-Phase, when two-phase is solid, Can different material surface come into full contact with to the key that then can reaction go on smoothly.Usually utilize paddling process, polishing, ball The methods of mill method, supersonic airstream method and microwave method realize that two-phase interface comes into full contact with, and wherein ball-milling method is a kind of feasible And efficient solid phase synthesis process.But usual ball milling is carried out in a locking device, is existed using steel ball or zirconia balls Its medium-high speed sports realizes the mixing dispersion of material, and material size very little in reaction process, dust is larger, if in reaction process In there are gas generations, then device internal pressure is larger, and reaction effect is bad.As lithium cell anode material of lithium iron phosphate utilizes phosphorus During sour iron and lithium carbonate ball-milling reaction, lithium carbonate, which is decomposed, generates lithia and carbon dioxide.Lithia and ball milling Solid phase reaction occurs for very thin ferric phosphate nucleus, and lithia gradually diffuses to ferric phosphate lattice and generates LiFePO4, can obtain The good LiFePO4 of size dispersity, but during the generation of great amount of carbon dioxide will cause ball-milling reaction in reaction process Dust disperses to be lost with lithia.Similar process is related to carbon there are also generation barium titanate etc. is reacted with barium carbonate using titanium dioxide The solid phase reaction that hydrochlorate participates in.
Based on this, the present invention devises consolidating for controlled release reaction gas on the basis of existing closed ball-milling device It is combined to reaction sphere grinding jar.
Summary of the invention
The present invention overcomes above-mentioned the deficiencies in the prior art, and providing one kind being capable of controlled release synthesis in solid state process generation gas The ball grinder of body.
To realize that the controllable purpose realized release reaction process and generate gas, the present invention adopt the following technical solutions:
A kind of ball-milling reaction tank, including cover, tank body and exhaust valve three parts.The successively row of installation at 1/4 position above the cover Air valve and pressure gauge.Exhaust valve mainly includes valve deck, the ball sealer with spring, fixture nut, filter membrane and a few part compositions of valve body. In sealing state, reacting powder and mill ball crushes in tank, the gas of generation flicks top valve ball when reaching certain pressure, Release gas.And the fine particle and dust wherein generated in reaction process reaches the mesh of gas solid separation by double layered cone funnel , micro fine dust is shut off by filter membrane, enters valve body in the case where high speed is shaken and participates in reaction.
The reaction vessel is stainless steel or polyurethane;
Compared with the prior art, the beneficial effects of the present invention are:
(1) controlled release that ball grinder of the present invention may be implemented to generate gas in reaction process is realized while gas is released The separation of gas and solid dust, avoids reactant from losing;
(2) ball grinder adaptability of the present invention is good, can be used for liquid and solid or solid and solid are anti-under grinding condition It answers, effective monitoring can be carried out to the reaction for generating gas by pressure gauge;
(3) ball grinder of the present invention is used directly for directly applying on the general milling apparatus such as planetary mills, concussion mill, especially suitable In the solid phase synthesis that carbonate participates in.
Detailed description of the invention
Fig. 1 is ball grinder overall structure diagram of the present invention;
Wherein, 1-tank body;2- official hats and canopies;3-vent valves;4-pressure gauges.
Fig. 2 is vent valve scheme of installation of the present invention:
Wherein, 1-valve deck;2- spring;3-ball sealers;4-gas vents;5-filter membrane nuts;6-valve bodies;7-fixators;8— Cover;9-sieve plates;10-is conical baffled;11- sieve pore;12- pressure gauge;13- pressure gauge mounting hole;14- Upper gasket;15- underlay Piece.
Fig. 3 is that vent valve of the present invention disassembles schematic diagram.
Fig. 4 is overall operation schematic diagram of the present invention.
Specific embodiment
With reference to the accompanying drawing, description of specific embodiments of the present invention, as shown in Figure 1, the invention discloses one The ball grinder, including tank body 1, cover 2, vent valve 3 and pressure gauge 4 etc. of gas are generated in kind controlled release mechanical milling process.Tank body It is aluminium oxide with cover material, agate, polyurethane, polytetrafluoroethylene (PTFE), polypropylene, silicon carbide, zirconium dioxide, tungsten carbide or stainless Steel.After the placement tank body 1 by material, reactant and abrasive material are put into tank body, cover 2 is covered, by Waste gate to envelope Closed state.After locking entire ball grinder, under rotation status, abrasive material and reactant are fully ground in tank body, when reacting in tank After gas reaches certain pressure, gas opens the ball sealer of 3 upper end of vent valve, releases gas.By being mounted on cover Pressure gauge can set the blow off pressure of vent valve and monitor the variation for entirely grinding pressure inside the tank in process of lapping.
Fig. 2 is scheme of installation of the vent valve in cover.Wherein 1. valve deck;2. spring;3. ball sealer;4. gas vent;5 Filter membrane nut;6. valve body;7. fixator;8. cover;9. upper gasket;10. conical baffled;11. sieve pore;12. pressure gauge;13. pressure Power table mounting hole;14. lower gasket;15. filter membrane.When work, abrading-ball and reactive material are in tank body because of the rotation of tank body and phase Mutual friction crushes, and material reacts during contacting with each other, and the gas generated in reaction process can carry dust in space It diffuses.When gas pressure reaches certain setting pressure, so that ball sealer 3 moves up on valve body, gas is passed through on cover Sieve pore 11, most of dust in gas will receive conical baffled 10 blocking and return in tank, and gas, will be thin by filter membrane 15 Small dust is isolated from tank, and gas is discharged from gas vent 4.
Valve body from structure with functionally say, 1,2,3 belongs to sealing element, can by the knob of valve deck 1 and the flexible of spring To control the size of blow off pressure;10,15 belong to the purpose for realizing that solid gas or liquid gas separate in mixture, prevent loss of material.7 For connection valve body and cover.11 sieve pores are integrated with cover, and abrading-ball is avoided to collide valve body during the work time.12 be pressure gauge, Gas pressure change in tank is monitored, whether monitoring valve body is blocked by powder.When pressure inside the tank increase, valve body fails to discharge in time When gas, valve deck is unclamped manually, handles valve body blockage problem by way of reverse ventilation or directly dismantling valve body.
Fig. 3 is body portion structure broken away view, and all parts are detachable and interchangeable, and part name is identical with Fig. 2.
About erection sequence and modular construction function declaration:
Filter membrane nut and conical baffled (top coupling part band external screw thread) are connected through a screw thread by the first step, are padded on the folder of centre Circle, filter membrane and lower gasket;
Second step, the whole filter membrane nut for connecting previous step are connect with the internal screw thread of 6 conical top of valve body;
In the groove of third step, the integral installation for connecting previous step into valve deck 2 with sieve pore 11, in place after, 6 bottom of valve body Portion can fit with the groove structure of valve deck 2;
4th step, fixing holder 7.Play fixed and sealing function for 7 pair 6;
The valve deck 1 for being connected with spring 2 and ball sealer 3 is connect by screw thread with valve body 6 by the 5th step;
6th step, will pressure gauge install cover 2 on mounting hole on.
The course of work (as shown in Figure 4): the reactant of certain material ratio is placed in tank body, covers and is connected with vent valve Cover 2, fix cover outside after tank body, using external gas source by pressure gauge installing port ventilation pressurization, pass through valve deck spiral shell Line adjusts vent valve blow off pressure, after adjusting in place, deflates.Pressure gauge is installed in the pressure gauge mounting hole of cover 2.Work as tank When body high speed rotation, reactant reacts in crushing process releases gas, and gas is released when reaching certain pressure from vent valve.Prison The variation of measuring pressure meter pressure, if pressure rises, vent valve is released without gas, is stopped operating, by adjusting valve deck screw thread or tearing open Solution valve body checks whether that powder blocks vent valve.If pressure inside the tank no longer rises for a long time, then it represents that reaction terminates, and stops turning It is dynamic.
Although above-mentioned be described a specific embodiment of the invention in conjunction with attached drawing, not to the scope of the present invention Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to It is still within the scope of the present invention to make the creative labor the various modifications or changes that can be made.

Claims (7)

1. a kind of solid phase synthesis ball grinder, it is characterised in that including tank body, cover, vent valve and pressure gauge;The cover With sieve pore groove and pressure gauge mounting hole;The vent valve include valve deck, spring, ball sealer, valve body, filter membrane nut, filter membrane, Gasket and conical baffled;The valve body is installed on the groove slot with sieve pore of cover, is screwed by fixator;It is described Pressure gauge is installed in the pressure gauge mounting hole on cover, is threadedly coupled.
2. solid phase synthesis ball grinder as described in claim 1, which is characterized in that cover groove has and cover one Air guide sieve pore prevents abrading-ball in tank from contacting vent valve;It is screwed between cover and vent valve by fixator.
3. vent valve as described in claim 1, which is characterized in that be connected through a screw thread between cover and valve body, using valve body with The rotation of screw thread adjusts the elastic of sealing.
4. the valve body as described in right 1, which is characterized in that valve body includes straight-tube portion and lower end conical section;Have in the middle part of straight tube Gas port, gas port joint are the groove that fits with ball sealer, and there is external screw thread in straight tube upper end, is connected with valve deck, pipe lower end Internal screw thread is connect with upper filter membrane clip, and lower end conical section taper is 30-150 °, and bottom edge fits with cover groove.
5. filter membrane nut as described in claim 1, which is characterized in that the interior spiral shell of filter membrane nut external screw thread and valve body straight tube lower part Line matches, and filter membrane nut inner thread is matched with conical baffled upper end coupling part internal screw thread, keeps off in filter membrane nut and taper Upper gasket, filter membrane and lower gasket are fixed between plate interconnecting piece.
6. it is as described in claim 1 it is conical baffled include, including top with externally threaded interconnecting piece lower part back taper aperture Following conical baffled top drilling is protruded into, is connected with below conical baffled by rib formula, conical baffled top drilling, taper It is 30-150 °.
7. fixator as described in claim 1, which is characterized in that external screw thread is connected with cover, under internal taper and valve body End toper fits.
CN201811040482.8A 2018-09-07 2018-09-07 A kind of solid phase synthesis ball grinder Pending CN109261295A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811040482.8A CN109261295A (en) 2018-09-07 2018-09-07 A kind of solid phase synthesis ball grinder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811040482.8A CN109261295A (en) 2018-09-07 2018-09-07 A kind of solid phase synthesis ball grinder

Publications (1)

Publication Number Publication Date
CN109261295A true CN109261295A (en) 2019-01-25

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Country Status (1)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112206879A (en) * 2020-09-15 2021-01-12 方国樟 Anti-overload pressure adjustable ball mill

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001334157A (en) * 2000-05-26 2001-12-04 Hitachi Cable Ltd Pulverizing method for powder by low-temperature vibration mill
CN203570710U (en) * 2013-07-09 2014-04-30 嘉兴博科精密机械有限公司 Automatic exhaust oil tank
CN203598873U (en) * 2013-11-29 2014-05-21 山东科技大学 Novel high pressure ball-milling tank
CN104549658A (en) * 2014-12-24 2015-04-29 华南理工大学 Application method of cold field plasma discharge assisted high energy ball milled powder and plasma assisted high energy ball milling device
CN204953020U (en) * 2015-08-25 2016-01-13 赣州长辉磁业有限公司 A grinder for magnetic material
CN205340944U (en) * 2016-02-02 2016-06-29 宜昌久久鑫建筑材料有限公司 A exhaust apparatus for wet ball mill
CN206229450U (en) * 2016-11-29 2017-06-09 四川建筑职业技术学院 A kind of ball mill
CN107413461A (en) * 2017-08-02 2017-12-01 嘉善县天成强磁有限责任公司 Ceramic ball mill
CN206868343U (en) * 2017-06-29 2018-01-12 瑞安市善源机械有限公司 Ball mill
CN207093032U (en) * 2017-07-07 2018-03-13 中国石油天然气股份有限公司 A kind of valve discharging gas under certain pressure

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001334157A (en) * 2000-05-26 2001-12-04 Hitachi Cable Ltd Pulverizing method for powder by low-temperature vibration mill
CN203570710U (en) * 2013-07-09 2014-04-30 嘉兴博科精密机械有限公司 Automatic exhaust oil tank
CN203598873U (en) * 2013-11-29 2014-05-21 山东科技大学 Novel high pressure ball-milling tank
CN104549658A (en) * 2014-12-24 2015-04-29 华南理工大学 Application method of cold field plasma discharge assisted high energy ball milled powder and plasma assisted high energy ball milling device
CN204953020U (en) * 2015-08-25 2016-01-13 赣州长辉磁业有限公司 A grinder for magnetic material
CN205340944U (en) * 2016-02-02 2016-06-29 宜昌久久鑫建筑材料有限公司 A exhaust apparatus for wet ball mill
CN206229450U (en) * 2016-11-29 2017-06-09 四川建筑职业技术学院 A kind of ball mill
CN206868343U (en) * 2017-06-29 2018-01-12 瑞安市善源机械有限公司 Ball mill
CN207093032U (en) * 2017-07-07 2018-03-13 中国石油天然气股份有限公司 A kind of valve discharging gas under certain pressure
CN107413461A (en) * 2017-08-02 2017-12-01 嘉善县天成强磁有限责任公司 Ceramic ball mill

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112206879A (en) * 2020-09-15 2021-01-12 方国樟 Anti-overload pressure adjustable ball mill

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Effective date of registration: 20200929

Address after: 271016 Shandong First Medical University (Shandong Academy of Medical Sciences)

Applicant after: Shandong First Medical University (Shandong Academy of Medical Sciences)

Address before: 271016 Chemistry and Pharmaceutical Engineering of Taishan Medical College, 619 Great Wall Road, Taian City, Shandong Province

Applicant before: TAISHAN MEDICAL University

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RJ01 Rejection of invention patent application after publication

Application publication date: 20190125

RJ01 Rejection of invention patent application after publication