CN206286558U - A kind of liquid phase slit interference synthesis device - Google Patents

Abstract

The utility model is related to a kind of liquid phase slit interference synthesis device, including the upper and lower two parallel flat restricted area of binary channels slit and single channel slit synthesis zone, fixation after connecting is inlayed with single channel slit synthesis zone convex-concave and is placed on AB areas linking fixed station in upper and lower two parallel flat restricted area of binary channels slit, the vertical plane of the single channel slit synthesis zone flat restricted area connecting portion of binary channels slit parallel with upper and lower two is ultrasonic device joint face, ultrasonic device joint face welding ultrasonic transmitter；The measuring tank that deenergizes is divided into liquid zone by the measuring tank dividing plate that deenergizes and goes out liquid zone, wherein enter liquid zone and connected in energy measuring tank dividing plate bottom with liquid zone is gone out, enter the silver powder taphole that the generation of single channel slit synthesis zone is accepted in liquid zone, go out liquid zone and filter washing equipment is connected by outlet at bottom.The equipment solves the concentration changes with time of stirred tank, stirs the synthesis mode that silver powder that is uneven, cannot synthesizing different grain size proportioning, microcosmic extreme portions only rely on surfactant, starts liquid phase high stability continuous high-end slurry silver powder controlling apparatus for synthesizing and method without back-mixing.

Description

A kind of liquid phase slit interference synthesis device

Technical field

The utility model belongs to liquid phase synthesis equipment technical field, and in particular to one kind is mainly met the tendency of in silver powder liquid phase synthesis Micron, the liquid phase slit interference synthesis device of nm regime.

Background technology

External middle and high end silver powder monopolizes domestic market, and domestic enterprise is reluctant to produce great amount of investment, domestic technique skill to silver powder Art breaks through and difficulty is matched with low side devices, and automaticity is low.More than 90% enterprise is main synthesis device, table with stirred tank Face activating agent is main control device, is aided with other specification control, stops control on a macroscopic level, has interior six side to stir Kettle, degree of mixing has significant improvement, but cannot still solve the building-up process of the irregular change of concentration changes with time, makes Process control difficulties are obtained, human factor is more, poor repeatability.And the silver powder that different grain size is matched is directly synthesized, it piles up compactness Height, slurry electric conductivity is superior, and slurry company of many country is matched by later stage different grain size, realizes the raising of size performance, but Traditional approach cannot realize the silver powder product of different grain size ratio collocation.Therefore slurry is broken through and is significantly faster than silver powder production, causes state Interior silver powder industry is progressive slow in nearly 10 years, and only low and middle-end silver powder occupies part domestic market, and remaining is all by external. High-end silver powder synthetic technology block abroad fails the incoming country, and raising equipment control technology and process synthetic method are badly in need of in the country Innovation utility model research, make domestic to enter high-end silver powder product industry.

Traditional synthesis reactor liquid phase synthesis process, its concentration changes with time and irregular change, and batch (-type) Synthesis mode so that silver powder synthesizes controllable ability, is poor stable and uniform, poor repeatability, it is impossible to enter high-end silver powder industry One of the main reasons, and cannot realize different grain size proportioning silver powder product.For the liquid phase synthesis for selecting system, urged in nothing In the case of agent, shown by orthogonal experiment, system reactant concentration is synthesis silver powder characteristic index influence most important factor, and The a large amount of of surfactant are used, and some electric properties of powder are reduced in terms of certain.

Utility model content

Technical problem to be solved in the utility model is directed to shortcoming of the prior art and provides a kind of liquid phase slit Interference synthesis device, the utility model aims to solve the problem that the brought influence of the irregular change of concentration, reduces making for surfactant Consumption, it is ensured that silver powder building-up process is microcosmic controllable, realizes continuous synthesis mode, improves silver powder items characteristic index, keeps height Repeatability, reaches that product is uniform and stable, and can realize being directly synthesized the silver powder of different grain size proportioning, starts liquid phase high stability company The continuous high-end silver powder synthesis control new method without back-mixing.

Adopted the following technical scheme that to solve technical problem of the present utility model：

A kind of liquid phase slit interference synthesis device, including upper and lower two parallel flat restricted area of binary channels slit and single channel Inlayed with single channel slit synthesis zone convex-concave and connected in slit synthesis zone, upper and lower two parallel flat restricted area of binary channels slit Fixation afterwards is placed on AB areas linking fixed station；Wherein upper and lower two parallel flat restricted area of binary channels slit are respectively equipped with oxidation also Raw material import and reduction-oxidation material import, the redox material inlet and the import of reduction-oxidation material can be close with prismatic Enclosed dosing kettle is connected；The single channel slit synthesis zone is the rectangle ghost that can lead to cooling circulating water, and the single channel is narrow It is stitched into part side of the area near the upper and lower two parallel flat restricted area of binary channels slit and is provided with cooling water inlet, opposite side sets Coolant outlet is put, insulation sleeve is cased with outside the single channel slit synthesis zone, the insulation sleeve top and bottom are provided with two and put down First electrode plate and second electrode plate can be bumped into and fixed by row of channels respectively, and the first electrode plate and second electrode plate are equal It is provided with the current controller binding post linked with current controller；The single channel slit synthesis zone and upper and lower two parallel bilaterals The vertical plane of the flat restricted area connecting portion of road slit is ultrasonic device joint face, and the ultrasonic device joint face welds ultrasound emission Device；The measuring tank that deenergizes is divided into liquid zone by the measuring tank dividing plate that deenergizes and goes out liquid zone, wherein entering liquid zone and going out liquid zone in energy measuring tank dividing plate Bottom connects, and enters the silver powder taphole that the generation of single channel slit synthesis zone is accepted in liquid zone, goes out liquid zone and is connected by outlet at bottom Filter washing equipment.

Upper and lower two parallel a length of 0.2m-5m in the flat restricted area of binary channels slit, wherein each passage slit is a width of 0.2m-1.5m, a height of 0.001m-0.5m.

The single channel slit synthesis zone（A）A length of 0.2m-5m, a width of 0.2m-1.5m, a height of 0.004m-1.002m.

The insulation sleeve is quality of rubber materials.

The utility model is carried out flat by a pair slit stack of shared reaction interval to liquid phase oxidation reducing solution Limitation, the electric field via current controller coordination electrode plate is interfered, and forms control interval, cooling circulating water cooling, ultrasound Under the mate-assist of controller, from microcosmic upper control anions and canons dynamic so that cation is as few as possible to be connect with reactor wall Touch, realize that cation carries out Spatial Multi-Dimensional rotation in slit space by horizontal pressure difference and electric field vertical distraction forced oscillation, reach To uniform sequential liquid phase micromanagement building-up process, and class laminar flow or to shake state propulsion and vertical is kept in the middle of slit Directional pull plays reciprocation with chemical reaction driving force, reaches the solution concentration on each vertical plane and does not change over time And change, maintain whole reaction interval concentration gradient constant.Reduction forms particulate matter and then departs from electric field controls, in horizontal pressure difference and Mixed zone end is flowed out under gravity and ultrasonication, the holding to reducing metal particle end state is realized by the measuring tank that deenergizes.Make Material solves synthesis reactor concentration changes with time and irregular change in the interval continuous synthesis mode for forming uniform rule of synthesis Purpose, and then realize that synthetic powder index is controllable, epigranular uniformity is good, or different grain size proportioning high duplication and electricity The raising of performance.When coordinating with certain reducing agent, the comprehensive covering from micron to nanometer is capable of achieving.The utility model is maximum The characteristics of be to be changed into micromanagement from traditional macro-control, and the reciprocation of active force so that the stabilization of indicator powder Property, the uniformity of granularity, electric property is greatly improved, and realizes that size distribution is interval adjustable, reduces part surface and lives Property agent consumption and low in energy consumption, put into suitable with traditional simplest equipment, realize entirely different and more stable controlling party Formula.From surfactant usage amount is reduced, product acquires very big economic benefit into the added value aspect of high-end market, By meeting the tendency of for slit interference synthetic technology, the continuous microcosmic controlledly synthesis of silver powder is realized, change silver powder synthesis device list One, concentration changes with time and change, control is discontinuous, and batch (-type) fluctuation is big, and cannot realize being directly synthesized different grain size silver The technical problem of powder proportioning.

Brief description of the drawings

Fig. 1 is the utility model structural representation；

Fig. 2 is the utility model single channel slit synthesis zone and first electrode plate and second electrode plate cooperation schematic diagram；

Fig. 3 is the utility model single channel slit synthesis zone structural representation；

Fig. 4 is the C-C sectional views of Fig. 3；

Fig. 5 is the parallel flat restricted area structural representation of binary channels slit of upper and lower two of the utility model；

Fig. 6 is the C-C sectional views of Fig. 5.

Specific embodiment

The utility model is described in further details below in conjunction with the accompanying drawings：

As shown in figures 1 to 6, a kind of liquid phase slit interference synthesis device, including upper and lower two parallel flat limits of binary channels slit Area B processed and single channel slit synthesis zone A, upper and lower two parallel flat restricted area B of binary channels slit and single channel slit synthesis zone （A）Fixation is placed on AB areas linking fixed station 3 after convex-concave inlays connection；Wherein upper and lower two parallel flat limitations of binary channels slit Area B is respectively equipped with redox material inlet 1 and reduction-oxidation material import 2, redox material inlet 1 and reduced oxide Material import 2 and prismatic can closed dosing kettle be connected；Single channel slit synthesis zone A is the rectangle sky that can lead to cooling circulating water Shell, single channel slit synthesis zone A is provided with cooling water near the part side of the upper and lower two parallel flat restricted area B of binary channels slit Import 4, opposite side sets coolant outlet 6, and insulation sleeve 11 is cased with outside single channel slit synthesis zone A, and insulation sleeve 11 is rubber Glue material matter.The top and bottom of insulation sleeve 11 are provided with battery lead plate jack, and first electrode plate 10 and second electrode plate 13 are bumped into edge insulator Set 11 is simultaneously fixed, and first electrode plate 10 and second electrode plate 13 are equipped with the current controller wiring linked with current controller Post；The vertical plane of the single channel slit synthesis zone A flat restricted area B connecting portions of binary channels slit parallel with upper and lower two is ultrasound Device joint face 12, ultrasonic transmitter is welded in ultrasonic device joint face 12；The measuring tank 9 that deenergizes is feed liquor by 8 points of the measuring tank dividing plate that deenergizes Area and go out liquid zone, wherein enter liquid zone and go out liquid zone being connected in the bottom of energy measuring tank dividing plate 8；Enter the silver that synthesis zone B generations are accepted in liquid zone Powder taphole, goes out liquid zone and connects filter washing equipment by outlet at bottom；Wherein upper and lower two parallel binary channels slits are flat The a length of 0.2m-5m of restricted area B, the wherein a width of 0.2m-1.5m of each passage slit, a height of 0.001m-0.5m, synthesis zone single channel Slit a length of 0.2m-5m, it is wide it is consistent with binary channels be 0.1m-1.5m, a height of single channel height of binary channels slit two extraordinarily The thickness in intermediate layer, is 0.004m-1.002m.Member principle and effect：The synthesis device be synthesis zone, flat restricted area, absolutely The assembly of edge cutting ferrule, battery lead plate, convenient dismounting cleaning.Insulating coating be mainly mixed zone set one section with battery lead plate phase The insulation set of matching.Battery lead plate is one or more pairs of electrodes corresponding with mixed zone horizontal plane and parallel, is respectively attached to Slit top and bottom, current controller can use commercially available VVVF systems, and more excellent selection direct current controls circuit by PLC time-program(me)s Break-make system, realizes that forward current replaces the continuous process of make-and-break time with reverse current, primarily serves coordination electrode two ends Size of current or size of current and direction cyclically-varying, to the interference effect of ionic reaction（Size of current and solution viscosity, from Sub-feature is associated）, it is possible to achieve cation has tractive force vertically upward in initial mixing area, is carried out after reaching certain altitude Vibrational control, can also realize that cation starts just to carry out vibrational control on each vertical plane in mixed zone, and the component is to realize The important component of epigranular or different grain size proportioning.Cooling circulating water is mainly offset mixed zone Liquid reduction reaction process and is produced in itself The unnecessary temperature of life, prevents constant temperature from raising, and mixed zone Ion transfer is had a negative impact.Ultrasonic transmitter is mainly pair also Former solid phase powder material plays cleaning, prevents from sticking to inner slit walls, produces the negative effect of accumulation.The quick measuring tank master that deenergizes Synthesis liquid is accepted for linking slot ends rise, and energy is quickly removed to the solution after synthesis, the purpose of stabilization liquid phase material.This Device and method are that, by silver nitrate, reducing agent, a small amount of surfactant is configured to two isometric component solutions, is divided to upper and lower two Layer, with certain flow rate by flat restricted area, in slit mixed zone, through overcurrent controller to the current control of battery lead plate, shape It is interval into electric field controls, can be an interval, or it is multiple interval, and then control liquid phase material ion dynamic and be distributed；It is logical Supercooling recirculated water prevents ion from varying with temperature generation Influence of Displacement, solution cation is kept class in the middle of slit vertical plane Laminar flow is advanced with oscillatory regime, and the active force realizes reciprocation with chemical reaction driving force, forms the dense of mixed zone stabilization Degree gradient, realizes that the concentration distribution on each vertical plane is not changed over time and changed, and reaching mixed zone concentration distribution short distance has Sequence, and reactive ion is gathered in slit central core and with upper bit formation reaction with chemical driving force and vibration conversion are automatic, should The then faint movement downwards under gravity of stage generation solid particle material, leaves with liquid stream by sonic oscillation, forms class A kind of uniform stable state building-up process of laminar flow, the solid mixed liquor for leaving enters the quick measuring tank that deenergizes, in the quick measuring tank that deenergizes Fast and stable liquid phase material is carried out, material is maintained at the state of mixed zone end, granular grows polymerization no longer occurs.The equipment And method emphasis is from the aspect of microcosmic, limited by slit is interval, orderly control of the electric field to microcosmic ion, and active force it Between reciprocation, solution concentration changes over time irregular change in solving Traditional liquid phase synthetic system.And active force Vibration and flow velocity passage and ultrasound and the mating reaction of measuring tank of deenergizing, the particle of generation is comparatively fast departed from reaction zone Between and stabilization, therefore the usage amount of part surface activating agent can be reduced in terms of certain.Accordingly when battery lead plate is carried out to reaction zone During zonal control, by matching for electric field level and direction change and solution concentration, then the liquid phase of different grain size proportioning can be realized Synthesis silver powder.The micromanagement of the utility model, realizes the maintenance of reaction system concentration gradient uniformity, and then ensure silver powder Building-up process is microcosmic controllable, forms continuous synthesis mode, improves silver powder items characteristic index, keeps high reproducibility, reaches Product granularity is uniform and stable or different grain size matches high duplication, realizes that the continuous high-end silver powder without back-mixing of liquid phase high stability is closed Into control new method.

During utility model works synthesis silver powder, finite concentration silver nitrate solution is first prepared, and add a small amount of surface-active Into solution I in prismatic dosing kettle, temperature control is between 20 DEG C -60 DEG C for dosage form；Prepare finite concentration reductant solution, reduction Agent can tentatively be matched according to silver powder index request, preferably normal temperature can occur the reducing agent for reducing silver nitrate, and add a small amount of surface Activating agent forms solution II in another prismatic dosing kettle, and temperature control is between 20 DEG C -60 DEG C；Synthesis starts, while opening molten The prismatic dosing kettle of liquid I and the prismatic dosing kettle of solution II go out hydraulic control valve, the correspondence of solution I flow into redox material inlet and Solution II is corresponded to and enters reduction-oxidation material import, unlatching cooling circulating water, unlatching ultrasonic transmitter, firing current controller, Solution I is this moment electric with solution II is by the flat restricted area B of parallel binary channels slit and then meets at single channel slit synthesis zone A Stream controller will converge reaction solution ion to the area carries out certain size of current, and mechanical periodicity control in direction forms microcosmic control The reaction of system；Solution leaves single channel slit synthesis zone A outlets after reaction, finally enters and has added half cold water to deenergize measuring tank 9 Enter liquid zone, when water temperature is higher than 20 DEG C, add water at low temperature to be cooled to less than 20 DEG C, when liquid level is high to the area, open energy measuring tank 9 Go out liquid zone bottom bleeder valve, silver powder mixed solution will be flowed into out liquid zone, and will be put into by bleeder valve by entering liquid zone by flashboard bottom Washing and filtering equipment carries out washing and filtering.Silver powder is finally entered into disk and enters vacuum drying oven, set 70 DEG C, dried, screening turns into terminal Silver powder product.When realizing that varigrained silver powder is matched simultaneously, then only single pair of battery lead plate need to be replaced with three pairs of divisional electrodes It is right, the periodic Control of different size of current is carried out respectively.

Claims (4)

1. a kind of liquid phase slit interference synthesis device, it is characterised in that：Including the upper and lower two parallel flat limitations of binary channels slit Area（B）With single channel slit synthesis zone（A）, upper and lower two parallel flat restricted area of binary channels slit（B）It is narrow with single channel It is stitched into area（A）Fixation is placed in AB areas linking fixed station after convex-concave inlays connection（3）On；Wherein upper and lower two parallel binary channels are narrow Stitch flat restricted area（B）It is respectively equipped with redox material inlet（1）With reduction-oxidation material import（2）, the redox Material inlet（1）With reduction-oxidation material import（2）With prismatic can closed dosing kettle be connected；The single channel slit synthesis zone （A）For the rectangle ghost of cooling circulating water, the single channel slit synthesis zone can be led to（A）Near upper and lower two parallel binary channels The flat restricted area of slit（B）Part side be provided with cooling water inlet（4）, opposite side setting coolant outlet（6）, the single-pass Road slit synthesis zone（A）It is cased with insulation sleeve outward（11）, the insulation sleeve（11）Top and bottom are provided with two parallel channels can Respectively by first electrode plate（10）With second electrode plate（13）It is bumped into and fixes, the first electrode plate（10）With second electrode plate （13）It is equipped with the current controller binding post linked with current controller；The single channel slit synthesis zone（A）With upper and lower two The individual parallel flat restricted area of binary channels slit（B）The vertical plane of connecting portion is ultrasonic device joint face（12）, the ultrasonic device company Junction（12）Welding ultrasonic transmitter；Deenergize measuring tank（9）By the measuring tank dividing plate that deenergizes（8）It is divided into liquid zone and goes out liquid zone, wherein Enter liquid zone and go out liquid zone in energy measuring tank dividing plate（8）Bottom connects, and enters liquid zone and accepts single channel slit synthesis zone（A）The silver powder of generation Taphole, goes out liquid zone and connects filter washing equipment by outlet at bottom.

2. a kind of liquid phase slit interference synthesis device according to claim 1, it is characterised in that：Described upper and lower two parallel The flat restricted area of binary channels slit（B）A length of 0.2m-5m, the wherein a width of 0.2m-1.5m of each passage slit, a height of 0.001m- 0.5m。

3. a kind of liquid phase slit interference synthesis device according to claim 1 and 2, it is characterised in that：The single channel is narrow It is stitched into area（A）A length of 0.2m-5m, a width of 0.2m-1.5m, a height of 0.004m-1.002m.

4. a kind of liquid phase slit interference synthesis device according to claim 3, it is characterised in that：The insulation sleeve（11） It is quality of rubber materials.