CN103658674A - Aqueous phase atmospheric pressure reduction kettle system for preparing Co-coated WC nanometer-assembly-structure composite powder - Google Patents

Aqueous phase atmospheric pressure reduction kettle system for preparing Co-coated WC nanometer-assembly-structure composite powder Download PDF

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Publication number
CN103658674A
CN103658674A CN201310715358.8A CN201310715358A CN103658674A CN 103658674 A CN103658674 A CN 103658674A CN 201310715358 A CN201310715358 A CN 201310715358A CN 103658674 A CN103658674 A CN 103658674A
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pressure reduction
reduction kettle
normal pressure
water
coated
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CN103658674B (en
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张璐
张忠健
张卫兵
彭奎
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Zhuzhou Cemented Carbide Group Co Ltd
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Zhuzhou Cemented Carbide Group Co Ltd
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Abstract

The invention discloses a new aqueous phase atmospheric pressure reduction kettle system for preparing Co-coated WC nanometer-assembly-structure composite powder. The aqueous phase atmospheric pressure reduction kettle system comprises an aqueous phase atmospheric pressure reduction kettle, a raw-material distribution system, a tail gas purification system and a washing suction filtration system, a water bath circulating temperature control system, a tail liquid processing system and an automatic control subsystem, the raw material distribution system, the tail gas purification system and the washing suction filtration system are connected with the feeding port, the exhausting port and the discharging port of the aqueous phase atmospheric pressure reduction kettle and are switched on and off under control of independent valves respectively, and the automatic control subsystem receives and process flow, pressure, electrical conductivity, temperature, light splitting luminosity meter and pH meter detection data of the systems and sends out control instructions. All components of the system work cooperatively, the complete processing system suitable for different processes is formed with the aid of automatic control procedure, the Co-coated WC nanometer-assembly-structure composite powder with stable quality can be produced efficiently and orderly, environmental pollution is avoided, and industrialization can be conducted efficiently and stably in an environmentally friendly mode.

Description

The water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co
Technical field
The present invention relates to hydrometallurgy and field of powder metallurgy, disclose the water normal pressure reduction kettle system of the coated WC nanometer package assembly composite powder of a kind of Co of preparation.
Background technology
With traditional in, coarse grain hard alloy compares, super thick, special coarse grain hard alloy has high thermal conductivity, thermal fatigue resistance and thermal shock resistance, have extremely wide application category preferably.Super thick, the special coarse grained carbide alloy of preparation is still a short slab of cemented carbide industry at present, existing many patents of invention propose the preparation method of coarse grain hard alloy at present, wherein carbide alloy industry renowned company adopts sol-gel (Sol-gel) legal system for coarse grained carbide alloy, but the required injection coating equipment technological requirement level of this technology is higher.
Patent CN201210046476.7 proposes to adopt normal pressure water reducing process to prepare the coated WC composite powder of super thick type Co, and this technology, based on organic matter reduction reaction mechanism, adopts extra-coarse grained WC material powder as heterogeneous nucleation core, adopts hydrazine hydrate N 2h 4h 2o is reducing agent, under normal pressure in 60 ~ 70 ℃ of reduction Co hydroxide water pastes; Adopt the mode stirring that WC material powder is suspended in slip, by heterogeneous nucleation effect, prepare the coated WC type composite powder of nanometer package assembly Co.This technology has obtained the controlled high-quality carbide alloy of grain grade by selection and the follow-up alloy preparation technology of WC raw material granularity, has stronger feasibility.This patent lays particular emphasis on the central principle that product is prepared in earlier stage, belong to laboratory blank technology, and imperfection, especially in suitability for industrialized production, inevitably there are the following problems: 1) lack raw material distributing system, in original laboratory technique, raw material substantially adopts manually and drips, and is difficult to realize homogeneous reaction and gentle control of material; 2) do not comprise the tail gas that reaction is produced, the treatment technology of tail washings, and this technology relates to acid, alkali etc. to environmentally hazardous substance, conducts oneself well to put to guarantee its feature of environmental protection as improper; 3) in product washing impurity-removing link, there is no relevant treatment and analytical equipment, can not directly to impurities ion concentration in final products, analyze, production efficiency is low, also cannot guarantee the stability of product.
Summary of the invention
Object of the present invention is mainly to address the above problem in order to overcome, a set of new preparation nanometer package assembly Co water normal pressure reduction kettle system of coated WC composite powder is provided, the collaborative work of system each several part, under automatic control program auxiliary, formation can adapt to the complete process system of different process requirement, can effective produce the coated WC nanometer package assembly composite powder of stay-in-grade Co, and further avoid environmental pollution, make this technology can high efficiency, stable, environmental protection carry out industrialization.
The water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co of the present invention, comprise water normal pressure reduction kettle, be connected and control respectively by independent valve raw material distributing system, exhaust gas purification system and the washing suction filtration system of on off operating mode with charging aperture, exhaust outlet, the discharging opening of water normal pressure reduction kettle; And the water-bath circulating temperature control system being connected for heat structure with the hot water jacket of water normal pressure reduction kettle; The tail washings treatment system being connected with washing suction filtration system leakage fluid dram with described exhaust gas purification system; Receive and process the pressure detecting data of flow and pressure detecting data in described raw material distributing system, exhaust gas purification system, the electrical conductivity of washing suction filtration system detects data the spectrophotometer of the flow of water-bath circulating temperature control system and temperature detection data, tail washings treatment system and pH meter detect Data Concurrent go out control instruction from control subsystem.
As improvement, the inwall of described water normal pressure reduction kettle is lining titanium material, and inner contained puddler, blanking ball valve and mechanical seal is lining teflon material.
Described raw material distributing system comprises an one end by two Fluid sprayers that charging aperture insertion water normal pressure reduction kettle is inner, the other end is connected with valve with compressed air gas source, several raw material storage tanks of water normal pressure reduction kettle; Two Fluid sprayers feed in raw material in water normal pressure reduction kettle in the mode that liquid charging stock atomization is sprayed into; From control subsystem, by regulating the power of former material conveying pump to control conveying flow, and control accordingly compressed-air actuated pressure and guarantee that raw material sprays in water normal pressure reduction kettle with the form of atomization.
The venturi spray structure that described exhaust gas purification system adopts can be formed certain negative pressure, the inner solubility tail gas producing of reduction kettle be siphoned away and sprayed into solution.
Described washing suction filtration system comprise one can to slip carry out dispersed flow and adopt washing tower body that the deionized water of adverse current washs, be arranged at the conductivity meter that washing tower body delivery port judges material washability and be connected with delivery port, the discharging opening of washing tower body clean slip is carried out to the vacuum filtration tank of Separation of Solid and Liquid, washing water outlet exports and enters tail washings treatment system from described vacuum filtration pot bottom; From control subsystem, receive the washing water outlet conductivity signal of described washing suction filtration system, when washing water outlet conductivity >25 μ s/cm, from control subsystem, send instruction, control slip and be delivered to washing tower body charging aperture to carry out circulation cleaning by washing tower body discharging opening, when washing water outlet conductivity≤25 μ s/cm, from control subsystem, send instruction, control slip and be delivered to vacuum filtration tank and carry out Separation of Solid and Liquid by washing tower body discharging opening.
As further improvement, described tail washings treatment system comprises can carry out the waste liquid tank of solution self-loopa and the auxiliary material groove being connected with waste liquid tank, is provided with that can determine may be to the spectrophotometer of the content of the chemical composition of environment and pH meter in tail washings in waste liquid tank; Spectrophotometer in control subsystem receives waste liquid tank and pH meter detect data, and control the valve between waste liquid tank and auxiliary material groove, add respective amount auxiliary material removal may to the chemical composition of environment and regulate tail washings pH value to reach can discharge standard.
Described raw material distributing system source of the gas is preferably compressed air; Described several raw material storage tanks are fitted with respectively corresponding conveyance conduit and valve, carry respectively different material; Before conveyance conduit transferring raw material, adopt electrical conductivity to be less than or equal to the washed with de-ionized water of 20 μ s/cm.
Because automatic control system can gather the data of each several part and countercharge, can pre-programmed technology controlling and process curve according to process requirements, drive system each several part of the present invention collaborative work, under automatic control program auxiliary, can effective produce the coated WC nanometer package assembly composite powder of stay-in-grade Co, formed the complete process system that can adapt to different process requirement, and further avoid environmental pollution, making water normal pressure reducing process prepare the technology of the coated WC nanometer package assembly composite powder of Co can high efficiency, stable, environmental protection carry out industrialization.
Accompanying drawing explanation
fig. 1 is that the water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co of the present invention forms schematic diagram;
Fig. 2 is the typical scan electromicroscopic photograph (3000 times) of the coated WC nanometer package assembly composite powder of the Co for preparing of the present invention.
The specific embodiment
below in conjunction with drawings and Examples, the invention will be further described.
The water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co of the present invention, comprise water normal pressure reduction kettle 1, be connected and control respectively by independent valve raw material distributing system 2, exhaust gas purification system 3 and the washing suction filtration system 4 of on off operating mode with charging aperture, exhaust outlet, the discharging opening of water normal pressure reduction kettle 1; And the water-bath circulating temperature control system 5 being connected for heat structure with the hot water jacket of water normal pressure reduction kettle 1; The tail washings treatment system 6 being connected with washing suction filtration system 4 leakage fluid drams with described exhaust gas purification system 3; The electrical conductivity that receives and process flow and pressure detecting data in described raw material distributing system 2, washing suction filtration system 4 detect data, the temperature detection data of water-bath circulating temperature control system 5, the spectrophotometer of tail washings treatment system 6 and pH meter detect Data Concurrent go out control instruction from control subsystem 7.
The inwall of water normal pressure reduction kettle 1 is lining titanium material, and inner contained puddler, blanking ball valve and mechanical seal is lining teflon material.
Raw material distributing system 2 comprises an one end by charging aperture insertion water normal pressure reduction kettle 1 inside of water normal pressure reduction kettle 1, two Fluid sprayers 8 that the other end is connected with valve with source of the gas (being preferably compressed air), several raw material storage tanks; Two Fluid sprayers 8 feed in raw material in water normal pressure reduction kettle 1 in the mode that liquid charging stock atomization is sprayed into; From control subsystem 7, by regulating the power of former material conveying pump to control conveying flow, and the pressure of controlling accordingly source of the gas guarantees that raw material sprays in water normal pressure reduction kettle 1 with the form of atomization.Different material storage tank is fitted with respectively corresponding conveyance conduit and valve, carries respectively different material.Before conveyance conduit transferring raw material, adopt electrical conductivity to be less than or equal to the washed with de-ionized water of 20 μ s/cm.
The venturi spray structure that exhaust gas purification system 3 adopts can be formed certain negative pressure, the inner solubility tail gas producing of reduction kettle 1 be siphoned away and sprayed into solution.
Washing suction filtration system 4 comprise one can to slip carry out dispersed flow and adopt washing tower body 9 that the deionized water of adverse current washs, be arranged at the conductivity meter 10 that washing tower body 9 delivery ports judge material washability and be connected with delivery port, the discharging opening of washing tower body 9 clean slip is carried out to the vacuum filtration tank 11 of Separation of Solid and Liquid, wash water outlet and enter tail washings treatment system 6 from described vacuum filtration tank 11 outlet at bottoms; The described washing water outlet conductivity signal that receives described washing suction filtration system 4 from control subsystem 7, when washing water outlet conductivity >25 μ s/cm, from control subsystem 7, send instruction, control slip and be delivered to washing tower body 9 charging apertures to carry out circulation cleaning by washing tower body 9 discharging openings, when washing water outlet conductivity≤25 μ s/cm, from control subsystem 7, send instruction, control slip and be delivered to vacuum filtration tank 11 and carry out Separation of Solid and Liquid by washing tower body 9 discharging openings.
Tail washings treatment system 6 comprises can carry out the waste liquid tank 12 of solution self-loopa and the auxiliary material groove 13 being connected with waste liquid tank 12, is provided with that can determine may be to the spectrophotometer of the content of the chemical composition of environment and pH meter in tail washings in waste liquid tank 12; Described spectrophotometer and the pH meter receiving in waste liquid tank 12 from control subsystem 7 detects data, and control the valve of 13 of waste liquid tank 12 and auxiliary material grooves, add the auxiliary material of respective amount remove may to the chemical composition of environment and regulate tail washings pH value to reach can discharge standard.
With WC powder, solubility cobalt salt (CoCl 2deng), liquid caustic soda (NaOH), hydrazine hydrate be raw material, by water normal pressure reduction kettle system, preparing the coated WC nanometer assembling of Co composite powder is example, further illustrates the operation of water normal pressure reduction kettle system of the present invention.
Related raw material is inputted by the charging aperture on water normal pressure reduction kettle 1 top, and wherein WC powder, liquid caustic soda directly add, and the mode that solubility cobalt salt, hydrazine hydrate adopt two Fluid sprayers 8 to spray into atomization adds.The exhaust gas purification system 3 that the tail gas that reaction produces is connected by the exhaust outlet with water normal pressure reduction kettle 1 top is taken away and is processed, its operation principle is to adopt venturi spray structure, use recirculated water to carry out suction and pumping spray to reaction end gas, solubility harmful components dissolving in it is entered in recirculated water, and the recirculated water after use is delivered to tail washings treatment system 6 and processes.
Whole reaction is for being suspended objects system, in the process of reaction, need to regulate according to the different phase of reaction temperature and the mixing speed of reaction, this function controls respectively the temperature of water-bath circulating temperature control system 5 by the programing function from control subsystem 7 and the stirring motor rotating speed of water normal pressure reduction kettle 1 is realized.After sufficient reacting completes, can automatically be cooled to room temperature and keep constant temperature and certain speed of agitator, making material system keep stable.
Material after reacting completely is delivered to washing suction filtration system 4 by the discharging opening of water normal pressure reduction kettle 1 bottom to carry out after washing impurity-removing, Separation of Solid and Liquid, finally obtains the coated WC nanometer package assembly composite powder of Co.The charging aperture of washing tower body 9 is positioned at tower body top, is connected with the discharging opening of water normal pressure reduction kettle 1 bottom.Tower body contains the rotatable cutting plate of some layers, and when material is entered after tower body by charging aperture, because self gravity drops down onto on cutting plate, cutting plate disperses material by rotation, and the material after dispersion drops down onto next stage cutting plate along taper tower wall.The water inlet of washing tower body 9 is positioned at the bottom of tower body, delivery port is positioned at the top of tower body, the direction of motion after deionized water enters is contrary with material, and the ion in the process of relative motion in material spreads fully and is pulled away, thereby reaches the object of washing material.The delivery port of washing tower body 9 disposes conductivity meter 10, can judge material washability.From control subsystem 7, receive the signal of conductivity meter 10, when washing water outlet conductivity >25 μ s/cm, from control subsystem 7, send instruction, control slip and be delivered to washing tower body 9 charging apertures to carry out circulation cleaning by washing tower body 9 discharging openings, when washing water outlet conductivity≤25 μ s/cm, from control subsystem 7, send instruction, control slip and be delivered to vacuum filtration tank 11 and carry out Separation of Solid and Liquid by washing tower body 9 discharging openings, obtain the coated WC nanometer package assembly composite powder of Co.In washing process, vacuum filtration tank 11 keeps work always, and washing water outlet is drawn into vacuum filtration tank 11 bottoms, then enters tail washings treatment system 6 by its outlet at bottom;
The mode that tail washings treatment system 6 adopts Threshold Analysis to process is processed waste water, by its built-in spectrophotometer and pH meter, can carry out quantitative analysis to harmful components (remaining hydrazine hydrate and liquid caustic soda), and feed data back to from control subsystem 7, when assay value reaches upper threshold, the valve of waste liquid tank 12 and auxiliary material groove 13 is opened in control, add the auxiliary material (oxidant and acid) of respective amount to process, it is reached can discharge standard.In the present embodiment, washing water outlet conductivity is 17-22 μ s/cm; N in tail washings after processing 2h 4content is 0.02mg/L, and pH value is 7, meets discharge standard.
The nanometer package assembly composite powder of the coated WC of Co preparing by water normal pressure reduction kettle system of the present invention, its stereoscan photograph as shown in Figure 2.Nano level Co powder is evenly distributed on around micron-sized WC particle as seen from the figure, forms the coated WC nanometer package assembly composite powder of Co.

Claims (9)

1. prepare the water normal pressure reduction kettle system that Co is coated the nanometer package assembly composite powder of WC for one kind, comprise water normal pressure reduction kettle (1), it is characterized in that also comprising the raw material distributing system (2), exhaust gas purification system (3) and the washing suction filtration system (4) that are connected with charging aperture, exhaust outlet, the discharging opening of water normal pressure reduction kettle (1) respectively and by independent valve, control respectively on off operating mode; And the water-bath circulating temperature control system (5) being connected for heat structure with the hot water jacket of water normal pressure reduction kettle (1); The tail washings treatment system (6) being connected with washing suction filtration system (4) leakage fluid dram with described exhaust gas purification system (3); The electrical conductivity that receives and process flow and pressure detecting data in described raw material distributing system (2), washing suction filtration system (4) detect data, the temperature detection data of water-bath circulating temperature control system (5), the spectrophotometer of tail washings treatment system (6) and pH meter detect Data Concurrent go out control instruction from control subsystem (7).
2. preparation Co according to claim 1 is coated the water normal pressure reduction kettle system of the nanometer package assembly composite powder of WC, the inwall that it is characterized in that described water normal pressure reduction kettle (1) is lining titanium material, and inner contained puddler, blanking ball valve and mechanical seal is lining teflon material.
3. the water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co according to claim 1, is characterized in that described raw material distributing system (2) comprises an one end by two Fluid sprayers (8) that charging aperture insertion water normal pressure reduction kettle (1) is inner, the other end is connected with valve with source of the gas, several raw material storage tanks of water normal pressure reduction kettle (1); Described two Fluid sprayers (8) feed in raw material in water normal pressure reduction kettle (1) in the mode that liquid charging stock atomization is sprayed into; Described from control subsystem (7) by regulating the power of former material conveying pump to control conveying flow, and the pressure of controlling accordingly source of the gas guarantees that raw material sprays in water normal pressure reduction kettle (1) with the form of atomization.
4. the water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co according to claim 1, is characterized in that described exhaust gas purification system (3) adopts the venturi spray structure that can form certain negative pressure, the inner solubility tail gas producing of reduction kettle (1) be siphoned away and sprayed into solution.
5. preparation Co according to claim 1 is coated the water normal pressure reduction kettle system of the nanometer package assembly composite powder of WC, it is characterized in that described washing suction filtration system (4) comprises one and can carry out the dispersed washing tower body (9) that flows and adopt the deionized water of adverse current to wash to slip, be arranged at the conductivity meter (10) that washing tower body (9) delivery port judges material washability, and with washing tower body (9) delivery port, the vacuum filtration tank (11) that clean slip is carried out to Separation of Solid and Liquid that discharging opening is connected, washing water outlet enters tail washings treatment system (6) from described vacuum filtration tank (11) outlet at bottom, the described washing water outlet conductivity signal that receives described washing suction filtration system (4) from control subsystem (7), when washing water outlet conductivity >25 μ s/cm, from control subsystem (7), send instruction, control slip and be delivered to washing tower body (9) charging aperture to carry out circulation cleaning by washing tower body (9) discharging opening, when washing water outlet conductivity≤25 μ s/cm, from control subsystem (7), send instruction, control slip and be delivered to vacuum filtration tank (11) and carry out Separation of Solid and Liquid by washing tower body (9) discharging opening.
6. preparation Co according to claim 1 is coated the water normal pressure reduction kettle system of the nanometer package assembly composite powder of WC, it is characterized in that described tail washings treatment system (6) comprises can carry out the waste liquid tank (12) of solution self-loopa and the auxiliary material groove (13) being connected with waste liquid tank (12), is provided with that can determine may be to the spectrophotometer of the content of the chemical composition of environment and pH meter in tail washings in waste liquid tank (12); Described spectrophotometer and pH meter in control subsystem (7) receives waste liquid tank (12) detects data, and control the valve between waste liquid tank (12) and auxiliary material groove (13), add the auxiliary material of respective amount remove may to the chemical composition of environment and regulate tail washings pH value to reach can discharge standard.
7. the water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co according to claim 3, is characterized in that described raw material distributing system (2) source of the gas is compressed air.
8. the water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co according to claim 3, is characterized in that described several raw material storage tanks are fitted with respectively corresponding conveyance conduit and valve, carry respectively different material.
9. the water normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co according to claim 8, is characterized in that adopting electrical conductivity to be less than or equal to the washed with de-ionized water of 20 μ s/cm before described conveyance conduit transferring raw material.
CN201310715358.8A 2013-12-23 2013-12-23 The aqueous phase normal pressure reduction kettle system of the nanometer package assembly composite powder of the coated WC of preparation Co Active CN103658674B (en)

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CN106312087A (en) * 2015-07-03 2017-01-11 王东 Nanometal particles and preparation method thereof
CN106424714A (en) * 2016-11-18 2017-02-22 中国矿业大学 Composite WC alloy powder and preparation method and application thereof

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