CN116441239A - A deacidification washing device and method for producing high-purity spherical graphite - Google Patents
A deacidification washing device and method for producing high-purity spherical graphite Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000010439 graphite Substances 0.000 title claims abstract description 68
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 68
- 238000005406 washing Methods 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000004744 fabric Substances 0.000 claims abstract description 88
- 239000000706 filtrate Substances 0.000 claims abstract description 53
- 238000005507 spraying Methods 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000463 material Substances 0.000 claims description 60
- 239000007788 liquid Substances 0.000 claims description 39
- 239000007921 spray Substances 0.000 claims description 25
- 230000007246 mechanism Effects 0.000 claims description 21
- 238000009826 distribution Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 238000005054 agglomeration Methods 0.000 claims description 9
- 230000002776 aggregation Effects 0.000 claims description 9
- 239000012209 synthetic fiber Substances 0.000 claims description 6
- 229920002994 synthetic fiber Polymers 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- -1 polypropylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 11
- 239000002351 wastewater Substances 0.000 abstract description 5
- 238000004537 pulping Methods 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract description 3
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 description 20
- 238000003860 storage Methods 0.000 description 18
- 238000000034 method Methods 0.000 description 13
- 230000018044 dehydration Effects 0.000 description 8
- 238000006297 dehydration reaction Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/14—Removing waste, e.g. labels, from cleaning liquid
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Filtration Of Liquid (AREA)
Abstract
Description
技术领域technical field
本发明涉及石墨化工提纯技术领域，具体涉及一种生产高纯球形石墨用脱酸洗涤装置、应用及其制备方法。The invention relates to the technical field of graphite chemical purification technology, in particular to a deacidification washing device for producing high-purity spherical graphite, its application and its preparation method.
背景技术Background technique
石墨及其深加工产品具有独特的润滑性、电热传导性、耐高温性、耐腐蚀性等特性，广泛应用于机械、冶金、耐火等领域。尤其是高纯石墨产品在新能源电池、核工业、高级密封等高端领域应用前景广阔。Graphite and its deep-processed products have unique lubricity, electrical and thermal conductivity, high temperature resistance, corrosion resistance and other characteristics, and are widely used in machinery, metallurgy, refractory and other fields. In particular, high-purity graphite products have broad application prospects in high-end fields such as new energy batteries, nuclear industry, and advanced sealing.
高纯石墨的制备方法主要分为两种：高温法、化学法。高温法是利用石墨在非氧化气氛下耐高温的特性，在高温(＞2500℃)条件下非石墨矿物气化挥发，达到石墨提纯目的。化学法是通过化学药剂与非石墨矿物反应溶解，再经洗涤去除，实现石墨提纯。高温法由于成本过高，实际生产中较少采用。目前相关生产企业多采用化学法，尤以氢氟酸法为主，一般为石墨原料首先与以氢氟酸为主的混合酸液反应，然后进行脱酸洗涤，再与以盐酸为主的混合酸液进行二次反应，再经脱酸洗涤，干燥，制得高纯石墨产品。The preparation methods of high-purity graphite are mainly divided into two types: high temperature method and chemical method. The high temperature method is to use the high temperature resistance of graphite in a non-oxidizing atmosphere, and to vaporize and volatilize non-graphite minerals under high temperature (>2500°C) conditions to achieve the purpose of graphite purification. The chemical method is to achieve graphite purification by reacting and dissolving chemical agents with non-graphite minerals, and then removing them by washing. Due to the high cost, the high temperature method is rarely used in actual production. At present, the relevant production enterprises mostly use chemical methods, especially the hydrofluoric acid method. Generally, graphite raw materials are first reacted with a mixed acid solution mainly composed of hydrofluoric acid, then deacidified and washed, and then mixed with a hydrofluoric acid-based mixed acid solution. The acid solution undergoes a secondary reaction, and then deacidified, washed, and dried to obtain high-purity graphite products.
化学法制备高纯石墨必须经过洗涤工艺处理，才能将杂质与石墨分离，得到高纯石墨产品。目前，高纯石墨制备过程中洗涤工艺段采用设备主要为板框压滤机、离心机、带式过滤机，通过挤压、离心方式使固液分离，经过多次反复化浆、脱水或直接进行淋水洗涤，将溶解的杂质清洗干净。现有洗涤工艺直接采用清水/纯净水直接进行洗涤，耗水量极大，给后期废水处理造成很大的压力。The preparation of high-purity graphite by chemical method must go through a washing process to separate impurities from graphite and obtain high-purity graphite products. At present, the equipment used in the washing process section of the high-purity graphite preparation process is mainly plate and frame filter presses, centrifuges, and belt filters. Solid-liquid separation is achieved by extrusion and centrifugation. Wash with water to remove dissolved impurities. The existing washing process directly uses clean water/pure water for washing, which consumes a lot of water and puts a lot of pressure on the later wastewater treatment.
板框压滤机和离心机都是间断性工作，即供入浆料后，进行脱酸、洗涤，或反复多次脱水、化浆，再脱水、再化浆，但最终洗涤干净后卸料时，脱水和卸料不能同时进行，需停机，这导致其单台设备产能受限。Both plate and frame filter press and centrifuge work intermittently, that is, after feeding the pulp, deacidification, washing, or repeated dehydration, pulping, dehydration, and pulping again, but finally unloading after washing When dehydration and unloading cannot be carried out at the same time, it needs to be shut down, which limits the capacity of a single device.
板框压滤机、离心机、带式过滤机在脱水过程中，都会形成一定厚度的料层。如果反复将料层取出化浆，操作麻烦，耗时长，工作效率低，且容易造成物料损失；如果直接泵入清水洗涤，由于料层有一定的厚度，清水经过料层时存在分布不均，甚至可能存在洗涤死角，造成洗涤用水量大，洗涤效果不好等诸多不利影响。采用常规的带式过滤机虽可以实现连续加料、脱水、洗涤、卸料，但脱水后产品的含水量相对较高，约为30％左右。而采用板框压滤机和离心机对高纯球形石墨产品脱水后物料的含水量约为20％左右。Plate and frame filter presses, centrifuges, and belt filters will form a material layer of a certain thickness during the dehydration process. If the material layer is repeatedly taken out of the slurry, the operation is cumbersome, time-consuming, low work efficiency, and easy to cause material loss; if it is directly pumped into clean water for washing, since the material layer has a certain thickness, there will be uneven distribution of clean water when passing through the material layer. There may even be dead corners for washing, resulting in a large amount of washing water, poor washing effect and many other adverse effects. Although the conventional belt filter can realize continuous feeding, dehydration, washing, and unloading, the water content of the dehydrated product is relatively high, about 30%. However, the water content of the high-purity spherical graphite product is about 20% after the plate and frame filter press and the centrifuge are used to dehydrate the product.
现有的洗涤工艺，都是直接加入清水，洗涤用水量大，生产1吨高纯球形石墨产品需消耗纯净水25吨左右。洗涤过程中，随着清水的持续注入，排出的废水浓度会越来越低，最终产品中的残留杂质含量达到设定要求即视为洗涤干净。因此，洗涤前期其实并非必须用清水，而可以对不同浓度的洗涤废水进行梯次循环利用，以减少洗涤用水量。The existing washing process is to directly add clean water, which consumes a lot of washing water. It takes about 25 tons of pure water to produce 1 ton of high-purity spherical graphite products. During the washing process, with the continuous injection of clean water, the concentration of the discharged wastewater will become lower and lower, and the residual impurity content in the final product will be deemed to be clean after reaching the set requirements. Therefore, it is not necessary to use clean water in the early stage of washing, but the washing wastewater with different concentrations can be recycled in stages to reduce the amount of washing water.
本发明旨在开发一种制备高纯石墨用的高效脱酸洗涤工艺及装置，使之更符合高纯石墨制备，降低洗涤耗水量，缓解废水处理压力，降低高纯石墨生产成本，具有广阔的应用前景。The present invention aims to develop a high-efficiency deacidification and washing process and device for preparing high-purity graphite, so that it is more suitable for the preparation of high-purity graphite, reduces washing water consumption, eases the pressure of wastewater treatment, and reduces the production cost of high-purity graphite. Application prospects.
发明内容Contents of the invention
本发明的目的是提供一种生产高纯球形石墨用脱酸洗涤装置及方法，使之更符合高纯石墨制备，通过洗涤废水梯次循环利用降低了单位产品耗水量，实现单台洗涤设备连续不间断运行，提高了单机生产能力，提高生产效率。The purpose of the present invention is to provide a deacidification washing device and method for producing high-purity spherical graphite, so that it is more suitable for the preparation of high-purity graphite, and the water consumption per unit of product is reduced through the cascade recycling of washing wastewater, so that a single washing equipment can be continuously used without washing. Intermittent operation improves the production capacity of a single machine and improves production efficiency.
为达到上述目的，本发明采用的技术方案是：一种生产高纯球形石墨用脱酸洗涤装置，包括机身、入料装置、滤布、真空装置和卸料装置；所述滤布通过张紧装置连接在所述机身上并绕机身运行；所述机身上设有若干工作段，每个工作段的下方均设有超声波装置，所述工作段的上方设有喷淋装置，相邻工作段之间设有滚轴装置，每个工作段收集的滤液分别存放；所述真空装置位于所述滤布的下方以使滤布上下方形成压差；所述入料装置和卸料装置分别位于机身的两端。In order to achieve the above object, the technical scheme adopted in the present invention is: a kind of deacidification and washing device for producing high-purity spherical graphite, comprising a fuselage, a feeding device, a filter cloth, a vacuum device and a discharge device; The tightening device is connected to the fuselage and runs around the fuselage; there are several working sections on the fuselage, an ultrasonic device is installed under each working section, and a spraying device is arranged above the working section. There is a roller device between adjacent working sections, and the filtrate collected by each working section is stored separately; the vacuum device is located under the filter cloth to form a pressure difference between the upper and lower sides of the filter cloth; the feeding device and discharge The feeding devices are located at both ends of the fuselage.
优选地，所述张紧装置包括若干滚轴，所述滤布缠绕在滚轴上，且滤布的首尾连接，实现连续循环运行；所述滤布的上端为工作端，下端为循环回收端，所述真空装置位于滤布工作端的下方。Preferably, the tensioning device includes several rollers, the filter cloth is wound on the rollers, and the end of the filter cloth is connected to realize continuous cycle operation; the upper end of the filter cloth is the working end, and the lower end is the recycling end , the vacuum device is located below the working end of the filter cloth.
优选地，所述滤布工作端的下方设置有橡胶带，所述橡胶带用于承托滤布，所述橡胶带通过两个辊筒连接在所述机身上并绕机身运行。Preferably, a rubber belt is provided below the working end of the filter cloth, the rubber belt is used to support the filter cloth, the rubber belt is connected to the fuselage through two rollers and runs around the fuselage.
上文中，由于滤布的强度相对较低且运行时滤布上有料层，运行较为困难，所以需要橡胶带承托滤布以便于滤布运行。In the above, because the strength of the filter cloth is relatively low and there is a material layer on the filter cloth during operation, the operation is more difficult, so the rubber belt is required to support the filter cloth to facilitate the operation of the filter cloth.
优选地，所述机身上还设有电机和转动机构，所述电机和转动机构带动辊筒转动，依靠摩擦力带动橡胶带、滤布运行，所述电机和转动机构的速率可调。Preferably, the machine body is also provided with a motor and a rotating mechanism, the motor and the rotating mechanism drive the roller to rotate, rely on friction to drive the rubber belt and the filter cloth to run, and the speed of the motor and the rotating mechanism is adjustable.
优选地，所述橡胶带上设置有若干凹槽和/或若干小孔。Preferably, the rubber belt is provided with several grooves and/or several small holes.
优选地，相邻工作段之间设置的每个所述滚轴装置均包括两个滚轴机构，两个滚轴机构分别位于所述滤布工作端的上方和下方。Preferably, each of the roller devices arranged between adjacent working sections includes two roller mechanisms, and the two roller mechanisms are respectively located above and below the working end of the filter cloth.
优选地，所述真空装置包括若干独立的腔体，所述腔体的数量与所述工作段的数量相同；所述喷淋装置的数量比所述工作段的数量少一个。Preferably, the vacuum device includes several independent cavities, and the number of the cavities is the same as the number of the working sections; the number of the spraying device is one less than the number of the working sections.
上文中，第一个所述工作段的上方不设有喷淋装置，其他工作段的上方均设有喷淋装置。In the above, no spraying device is provided above the first working section, and spraying devices are provided above the other working sections.
优选地，每个所述腔体处均设有真空罐、真空泵和滤液收集口，所述滤液收集口通过管道与真空罐、真空泵相连接，所述真空泵运行产生负压；每个所述腔体内的滤液收集口分别收集其对应工作段的滤液，并分别存放。Preferably, each of the cavities is provided with a vacuum tank, a vacuum pump and a filtrate collection port, and the filtrate collection port is connected with the vacuum tank and the vacuum pump through a pipeline, and the operation of the vacuum pump generates negative pressure; each of the cavities The filtrate collection port in the body collects the filtrate of the corresponding working section respectively and stores them separately.
优选地，每个滤液收集口均通过管道连接有一个废液存储容器，滤液由滤液收集口排出进入真空罐，再经管道进入相应的废液存储容器。Preferably, each filtrate collection port is connected to a waste liquid storage container through a pipeline, and the filtrate is discharged from the filtrate collection port into the vacuum tank, and then enters the corresponding waste liquid storage container through the pipe.
优选地，前一个工作段上的喷淋装置与其后方工作段上的废液存储容器连通，并将后方工作段中的废液存储容器中的废液通入前一个工作段上的喷淋装置中，即前段喷淋用后段滤液；最后一个工作段上的喷淋装置采用纯净水。Preferably, the spray device on the previous working section communicates with the waste liquid storage container on the rear working section, and passes the waste liquid in the waste liquid storage container in the rear working section to the spray device on the previous working section In the middle, the filtrate in the back stage is used for the front stage spraying; the spray device on the last working stage uses pure water.
优选地，每个所述腔体内的真空度、每个所述超声波装置的超声波强度、每个所述滚轴装置之间的间距、每个滚轴装置中的两个滚轴机构之间的距离，喷淋装置中的喷淋水流量均可调节。Preferably, the degree of vacuum in each cavity, the ultrasonic intensity of each ultrasonic device, the distance between each roller device, and the distance between two roller mechanisms in each roller device The distance and the spray water flow in the spray device can be adjusted.
优选地，所述滤布为带式滤布，所述。滤布由合成纤维编织而成；所述合成纤维包括涤纶和丙纶。Preferably, the filter cloth is a belt filter cloth, the. The filter cloth is woven from synthetic fibers; the synthetic fibers include polyester and polypropylene.
优选地，所述机身除主要受力构件部分采用钢材外涂覆防腐材料，非受力或弱受力部分采用工程塑料材质。Preferably, the fuselage is coated with anti-corrosion materials except that the main force-bearing components are made of steel, and the non-stressed or weakly stressed parts are made of engineering plastics.
优选地，所述卸料装置包括卸料机构和刮板，洗涤干净的物料通过卸料机构卸出，少量粘在滤布上的残留物料由刮板去除。Preferably, the discharge device includes a discharge mechanism and a scraper, the cleaned material is discharged through the discharge mechanism, and a small amount of residual material stuck to the filter cloth is removed by the scraper.
上文中，所述机身上设有6个工作段，从靠近入料装置处至靠近卸料装置处分别为工作段A、工作段B、工作段C、工作段D、工作段E、工作段F，每个所述工作段之间的距离相同或不同，所述真空装置也分隔为6个相互独立的腔体；所述喷淋装置位于工作段B、工作段C、工作段D、工作段E、工作段F的上方，浓酸液在工作段A处过滤、收集，滤液由工作段A处的滤液收集口排出进入真空罐，再经管道进入相应的废液存储容器；工作段B上方的喷淋装置中的喷淋水使用工作段C处的废液存储容器收集的滤液、工作段C上方的喷淋装置中的喷淋水使用工作段D处的废液存储容器收集的滤液、工作段D上方的喷淋装置中的喷淋水使用工作段E处的废液存储容器收集的滤液、工作段E上方的喷淋装置中的喷淋水使用工作段F处的废液存储容器收集的滤液、工作段F上方的喷淋装置中的喷淋水使用纯净水。In the above, there are 6 working sections on the fuselage, which are working section A, working section B, working section C, working section D, working section E, working section from near the feeding device to near the unloading device. Section F, the distance between each of the working sections is the same or different, and the vacuum device is also divided into 6 mutually independent cavities; the spraying device is located in working section B, working section C, working section D, Above the working section E and working section F, the concentrated acid liquid is filtered and collected at the working section A, and the filtrate is discharged from the filtrate collection port at the working section A into the vacuum tank, and then enters the corresponding waste liquid storage container through the pipeline; the working section The spray water in the spray device above B uses the filtrate collected by the waste liquid storage container at the working section C, and the spray water in the spray device above the working section C uses the waste liquid storage container collected at the working section D The filtrate, the spray water in the spraying device above the working section D uses the filtrate collected by the waste liquid storage container at the working section E, and the spray water in the spraying device above the working section E uses the waste liquid at the working section F The filtrate collected in the storage container and the spray water in the spray device above the working section F use pure water.
本申请还要求保护一种生产高纯球形石墨用脱酸洗涤方法，采用上文所述的生产高纯球形石墨用脱酸洗涤装置，包括以下步骤：This application also claims to protect a method for deacidifying and washing the production of high-purity spherical graphite, using the above-mentioned deacidifying and washing device for producing high-purity spherical graphite, including the following steps:
S 1、装置运行，石墨浆料通过设置在机身一端的入料装置处供入，并均匀分布在滤布上；S 1. The device is running, and the graphite slurry is fed through the feeding device at one end of the fuselage, and evenly distributed on the filter cloth;
S2、浓酸液在第一个工作段处过滤、收集，滤液由滤液收集口排出进入真空装置中并收集，在第一个工作段处设置的超声波装置的超声波作用下，滤布上物料产生振动，使石墨粉分布更均匀，避免局部团聚形成包裹导致液体难以分离；S2. The concentrated acid liquid is filtered and collected at the first working section, and the filtrate is discharged from the filtrate collection port into the vacuum device and collected. Under the ultrasonic action of the ultrasonic device installed at the first working section, the material on the filter cloth is Vibration makes the graphite powder more evenly distributed and avoids local agglomeration to form packages that make it difficult to separate liquids;
S3、滤布运行将石墨运送至滚轴装置处，所述滚轴装置削去石墨分布不均造成的局部突起，使物料厚度保持均匀一致，物料通过滚轴装置时受到挤压有助于水分的脱除；S3. The filter cloth runs to transport the graphite to the roller device. The roller device cuts off the local protrusions caused by the uneven distribution of graphite, so that the thickness of the material is kept uniform. When the material passes through the roller device, it is squeezed to help moisture removal of
S4、物料通过滚轴装置后移动至下一工作段中，该工作段上方的喷淋装置对物料进行喷淋，经滤布过滤后，真空装置对滤液进行收集，设置的超声波装置的超声波作用下，滤布上物料产生振动，使石墨粉分布更均匀，避免局部团聚形成包裹导致液体难以分离；S4. The material moves to the next working section after passing through the roller device. The spraying device above the working section sprays the material. After filtering through the filter cloth, the vacuum device collects the filtrate. Next, the material on the filter cloth vibrates to make the graphite powder more evenly distributed and avoid partial agglomeration to form a package that makes it difficult to separate the liquid;
S5、滤布运行将石墨运送至下一个滚轴装置处，所述滚轴装置削去石墨分布不均造成的局部突起，使物料厚度保持均匀一致，物料通过滚轴装置时受到挤压有助于水分的脱除；S5. The filter cloth runs to transport the graphite to the next roller device. The roller device cuts off the local protrusions caused by the uneven distribution of graphite, so that the thickness of the material is kept uniform. When the material passes through the roller device, it is squeezed to help in the removal of moisture;
S6、物料通过S4中的滚轴装置后移动至下一工作段中，重复步骤S4-S5，直至物料在所有的工作段均已完成过滤；S6. The material is moved to the next working section after passing through the roller device in S4, and steps S4-S5 are repeated until the material has been filtered in all working sections;
S7、洗涤干净的物料在机身另一端的卸料装置中卸出；S7. The cleaned materials are unloaded from the unloading device at the other end of the fuselage;
步骤S4-S6中，所述工作段上方的喷淋装置采用的喷淋水为其后方工作段中收集的滤液，最后一个工作段上方的喷淋装置采用的喷淋水为纯净水。In steps S4-S6, the spraying water used by the spraying device above the working section is the filtrate collected in the working section behind it, and the spraying water used by the spraying device above the last working section is pure water.
上文中，滚轴装置不仅可以使物料厚度保持均匀一致，以便于后面喷淋、洗涤效果的均匀性，同时可将滤布分隔为不同的工作段，避免不同工作段的液体交叉。In the above, the roller device can not only keep the thickness of the material uniform, so as to facilitate the uniformity of the subsequent spraying and washing effects, but also divide the filter cloth into different working sections to avoid the liquid crossing in different working sections.
由于上述技术方案运用，本发明与现有技术相比具有下列优点：Due to the use of the above-mentioned technical solutions, the present invention has the following advantages compared with the prior art:
1.本发明开发了一种适合高纯球形石墨制备的脱水设备，该设备由一端加料另一端出料，可连续不间断运行，无需反复化浆脱水，提高单台洗涤脱水设备生产能力，提高生产效率，滤饼水分可控制在20％～25％。1. The present invention has developed a dehydration equipment suitable for the preparation of high-purity spherical graphite. The equipment feeds from one end and discharges from the other. It can run continuously without repeated pulping and dehydration, improving the production capacity of a single washing and dehydrating equipment. Production efficiency, filter cake moisture can be controlled at 20% to 25%.
2.本发明采用开发一种球形石墨用脱水洗涤工艺，在保证洗涤效果的前提下，通过洗涤废水梯次循环利用降低高纯球形石墨制备过程中的洗涤用水量，吨产品耗水量由30吨降低至8吨左右，降低能源消耗。2. The present invention adopts the development of a dehydration washing process for spherical graphite. Under the premise of ensuring the washing effect, the washing water consumption in the preparation process of high-purity spherical graphite is reduced through cascade recycling of washing wastewater, and the water consumption per ton of product is reduced by 30 tons. to about 8 tons, reducing energy consumption.
3.本发明通过滚轴装置将滤布分为多个工作段，通过滚轴装置保证多个工作段之间相互独立，避免不同工作段的液体交叉，可以使物料厚度保持均匀一致，以便于后面喷淋、洗涤效果的均匀性。3. The present invention divides the filter cloth into multiple working sections through the roller device. The roller device ensures that the multiple working sections are independent of each other, avoids the liquid crossing in different working sections, and can keep the thickness of the material uniform, so as to facilitate Uniformity of subsequent spraying and washing effects.
4、本发明在滤布工作段下方设置超声波装置，在超声波作用下，滤布上物料产生振动，使球形石墨粉分布更均匀，避免局部团聚形成包裹导致液体难以分离。4. In the present invention, an ultrasonic device is installed under the working section of the filter cloth. Under the action of ultrasonic waves, the material on the filter cloth vibrates to make the distribution of spherical graphite powder more uniform and avoid partial agglomeration to form packages that make it difficult to separate the liquid.
附图说明Description of drawings
为了更清楚地说明本发明具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单的介绍，显而易见地，下面描述中的一些附图是本发明的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings that need to be used in the description of the specific embodiments or prior art. Obviously, some of the following descriptions The accompanying drawings are some embodiments of the present invention, and those skilled in the art can obtain other accompanying drawings based on these drawings without any creative effort.
图1为本发明一种实施例的结构示意图。Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
图2为本发明一种实施例中机身与真空装置连接图。Fig. 2 is a connection diagram of the fuselage and the vacuum device in an embodiment of the present invention.
图3为本发明实施例三的结构示意图。Fig. 3 is a schematic structural diagram of Embodiment 3 of the present invention.
其中，1、机身；2、入料装置；3、滤布；4、真空装置；5、卸料装置；6、张紧装置；7、工作段；8、超声波装置；9、喷淋装置；10、滚轴装置；11、橡胶带；12、辊筒；13、刮板；41、真空罐；42、滤液收集口；Among them, 1. Fuselage; 2. Feeding device; 3. Filter cloth; 4. Vacuum device; 5. Unloading device; 6. Tensioning device; 7. Working section; 8. Ultrasonic device; 9. Spraying device ;10, roller device; 11, rubber belt; 12, roller; 13, scraper; 41, vacuum tank; 42, filtrate collection port;
71、工作段A；72、工作段B；73、工作段C；74、工作段D；75、工作段E；76、工作段F。71. Working section A; 72. Working section B; 73. Working section C; 74. Working section D; 75. Working section E; 76. Working section F.
具体实施方式Detailed ways
下面将结合附图对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions of the present invention will be clearly and completely described below in conjunction with the accompanying drawings. Apparently, the described embodiments are part of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例一Embodiment one
如图1-图2所示，本实施例涉及一种生产高纯球形石墨用脱酸洗涤装置，包括机身1、入料装置2、滤布3、真空装置4和卸料装置5；所述滤布通过张紧装置6连接在所述机身上并绕机身运行；所述机身上设有若干工作段7，每个工作段的下方均设有超声波装置8，所述工作段的上方设有喷淋装置9，相邻工作段之间设有滚轴装置10，每个工作段收集的滤液分别存放；所述真空装置位于所述滤布的下方以使滤布上下方形成压差；所述入料装置和卸料装置分别位于机身的两端。As shown in Figures 1-2, the present embodiment relates to a deacidification washing device for producing high-purity spherical graphite, including a fuselage 1, a feeding device 2, a filter cloth 3, a vacuum device 4 and a discharge device 5; The filter cloth is connected to the fuselage through a tensioning device 6 and runs around the fuselage; several working sections 7 are arranged on the fuselage, and an ultrasonic device 8 is arranged below each working section. Spraying device 9 is provided above the upper part, and roller device 10 is provided between adjacent working sections, and the filtrate collected in each working section is stored separately; the vacuum device is located below the filter cloth so that the upper and lower parts of the filter cloth form a Pressure difference; the feeding device and the discharging device are respectively located at the two ends of the fuselage.
优选地，所述张紧装置包括若干滚轴，所述滤布缠绕在滚轴上，且滤布的首尾连接，实现连续循环运行；所述滤布的上端为工作端，下端为循环回收端，所述真空装置位于滤布工作端的下方。Preferably, the tensioning device includes several rollers, the filter cloth is wound on the rollers, and the end of the filter cloth is connected to realize continuous cycle operation; the upper end of the filter cloth is the working end, and the lower end is the recycling end , the vacuum device is located below the working end of the filter cloth.
优选地，所述滤布工作端的下方设置有橡胶带11，所述橡胶带用于承托滤布，所述橡胶带通过两个辊筒12连接在所述机身上并绕机身运行。Preferably, a rubber belt 11 is provided below the working end of the filter cloth, the rubber belt is used to support the filter cloth, the rubber belt is connected to the fuselage through two rollers 12 and runs around the fuselage.
上文中，由于滤布的强度相对较低且运行时滤布上有料层，运行较为困难，所以需要橡胶带承托滤布以便于滤布运行。In the above, because the strength of the filter cloth is relatively low and there is a material layer on the filter cloth during operation, the operation is more difficult, so the rubber belt is required to support the filter cloth to facilitate the operation of the filter cloth.
优选地，所述机身上还设有电机和转动机构，所述电机和转动机构带动辊筒转动，依靠摩擦力带动橡胶带、滤布运行，所述电机和转动机构的速率可调。Preferably, the machine body is also provided with a motor and a rotating mechanism, the motor and the rotating mechanism drive the roller to rotate, rely on friction to drive the rubber belt and the filter cloth to run, and the speed of the motor and the rotating mechanism is adjustable.
优选地，所述橡胶带上设置有若干凹槽和/或若干小孔。Preferably, the rubber belt is provided with several grooves and/or several small holes.
优选地，相邻工作段之间设置的每个所述滚轴装置均包括两个滚轴机构，两个滚轴机构分别位于所述滤布工作端的上方和下方。Preferably, each of the roller devices arranged between adjacent working sections includes two roller mechanisms, and the two roller mechanisms are respectively located above and below the working end of the filter cloth.
优选地，所述真空装置包括若干独立的腔体，所述腔体的数量与所述工作段的数量相同；所述喷淋装置的数量比所述工作段的数量少一个。Preferably, the vacuum device includes several independent cavities, and the number of the cavities is the same as the number of the working sections; the number of the spraying device is one less than the number of the working sections.
上文中，第一个所述工作段的上方不设有喷淋装置，其他工作段的上方均设有喷淋装置。In the above, no spraying device is provided above the first working section, and spraying devices are provided above the other working sections.
优选地，每个所述腔体处均设有真空罐41、真空泵和滤液收集口42，所述滤液收集口通过管道与真空罐、真空泵相连接，所述真空泵运行产生负压；每个所述腔体内的滤液收集口分别收集其对应工作段的滤液，并分别存放。Preferably, each cavity is provided with a vacuum tank 41, a vacuum pump and a filtrate collection port 42, and the filtrate collection port is connected with the vacuum tank and the vacuum pump through a pipeline, and the operation of the vacuum pump generates negative pressure; The filtrate collection ports in the cavity respectively collect the filtrates of the corresponding working sections and store them separately.
优选地，每个滤液收集口均通过管道连接有一个废液存储容器，滤液由滤液收集口排出进入真空罐，再经管道进入相应的废液存储容器。Preferably, each filtrate collection port is connected to a waste liquid storage container through a pipeline, and the filtrate is discharged from the filtrate collection port into the vacuum tank, and then enters the corresponding waste liquid storage container through the pipe.
优选地，前一个工作段上的喷淋装置与其后方工作段上的废液存储容器连通，并将后方工作段中的废液存储容器中的废液通入前一个工作段上的喷淋装置中，即前段喷淋用后段滤液；最后一个工作段上的喷淋装置采用纯净水。Preferably, the spray device on the previous working section communicates with the waste liquid storage container on the rear working section, and passes the waste liquid in the waste liquid storage container in the rear working section to the spray device on the previous working section In the middle, the filtrate in the back stage is used for the front stage spraying; the spray device on the last working stage uses pure water.
优选地，每个所述腔体内的真空度、每个所述超声波装置的超声波强度、每个所述滚轴装置之间的间距、每个滚轴装置中的两个滚轴机构之间的距离，喷淋装置中的喷淋水流量均可调节。Preferably, the degree of vacuum in each cavity, the ultrasonic intensity of each ultrasonic device, the distance between each roller device, and the distance between two roller mechanisms in each roller device The distance and the spray water flow in the spray device can be adjusted.
优选地，所述滤布为带式滤布，所述。滤布由合成纤维编织而成；所述合成纤维包括涤纶和丙纶。Preferably, the filter cloth is a belt filter cloth, the. The filter cloth is woven from synthetic fibers; the synthetic fibers include polyester and polypropylene.
优选地，所述机身除主要受力构件部分采用钢材外涂覆防腐材料，非受力或弱受力部分采用工程塑料材质。Preferably, the fuselage is coated with anti-corrosion materials except that the main force-bearing components are made of steel, and the non-stressed or weakly stressed parts are made of engineering plastics.
优选地，所述卸料装置包括卸料机构和刮板13，洗涤干净的物料通过卸料机构卸出，少量粘在滤布上的残留物料由刮板去除。Preferably, the discharge device includes a discharge mechanism and a scraper 13, the cleaned material is discharged through the discharge mechanism, and a small amount of residual material stuck to the filter cloth is removed by the scraper.
实施例二Embodiment two
本实施例是在上述实施例一的基础上进行的，与上述实施例一相同之处不予赘述。This embodiment is carried out on the basis of the first embodiment above, and the similarities with the first embodiment will not be repeated.
本实施例涉及一种生产高纯球形石墨用脱酸洗涤方法，采用实施例一所述的生产高纯球形石墨用脱酸洗涤装置，包括以下步骤：This embodiment relates to a method for deacidifying and washing the production of high-purity spherical graphite, using the deacidifying and washing device for producing high-purity spherical graphite described in Example 1, comprising the following steps:
S 1、装置运行，石墨浆料通过设置在机身一端的入料装置处供入，并均匀分布在滤布上；S 1. The device is running, and the graphite slurry is fed through the feeding device at one end of the fuselage, and evenly distributed on the filter cloth;
S2、浓酸液在第一个工作段处过滤、收集，滤液由滤液收集口排出进入真空装置中并收集，在第一个工作段处设置的超声波装置的超声波作用下，滤布上物料产生振动，使石墨粉分布更均匀，避免局部团聚形成包裹导致液体难以分离；S2. The concentrated acid liquid is filtered and collected at the first working section, and the filtrate is discharged from the filtrate collection port into the vacuum device and collected. Under the ultrasonic action of the ultrasonic device installed at the first working section, the material on the filter cloth is Vibration makes the graphite powder more evenly distributed and avoids local agglomeration to form packages that make it difficult to separate liquids;
S3、滤布运行将石墨运送至滚轴装置处，所述滚轴装置削去石墨分布不均造成的局部突起，使物料厚度保持均匀一致，物料通过滚轴装置时受到挤压有助于水分的脱除；S3. The filter cloth runs to transport the graphite to the roller device. The roller device cuts off the local protrusions caused by the uneven distribution of graphite, so that the thickness of the material is kept uniform. When the material passes through the roller device, it is squeezed to help moisture removal of
S4、物料通过滚轴装置后移动至下一工作段中，该工作段上方的喷淋装置对物料进行喷淋，经滤布过滤后，真空装置对滤液进行收集，设置的超声波装置的超声波作用下，滤布上物料产生振动，使石墨粉分布更均匀，避免局部团聚形成包裹导致液体难以分离；S4. The material moves to the next working section after passing through the roller device. The spraying device above the working section sprays the material. After filtering through the filter cloth, the vacuum device collects the filtrate. Next, the material on the filter cloth vibrates to make the graphite powder more evenly distributed and avoid partial agglomeration to form a package that makes it difficult to separate the liquid;
S5、滤布运行将石墨运送至下一个滚轴装置处，所述滚轴装置削去石墨分布不均造成的局部突起，使物料厚度保持均匀一致，物料通过滚轴装置时受到挤压有助于水分的脱除；S5. The filter cloth runs to transport the graphite to the next roller device. The roller device cuts off the local protrusions caused by the uneven distribution of graphite, so that the thickness of the material is kept uniform. When the material passes through the roller device, it is squeezed to help in the removal of moisture;
S6、物料通过S4中的滚轴装置后移动至下一工作段中，重复步骤S4-S5，直至物料在所有的工作段均已完成过滤；S6. The material is moved to the next working section after passing through the roller device in S4, and steps S4-S5 are repeated until the material has been filtered in all working sections;
S7、洗涤干净的物料在机身另一端的卸料装置中卸出；S7. The cleaned materials are unloaded from the unloading device at the other end of the fuselage;
步骤S4-S6中，所述工作段上方的喷淋装置采用的喷淋水为其后方工作段中收集的滤液，最后一个工作段上方的喷淋装置采用的喷淋水为纯净水。In steps S4-S6, the spraying water used by the spraying device above the working section is the filtrate collected in the working section behind it, and the spraying water used by the spraying device above the last working section is pure water.
上文中，滚轴装置不仅可以使物料厚度保持均匀一致，以便于后面喷淋、洗涤效果的均匀性，同时可将滤布分隔为不同的工作段，避免不同工作段的液体交叉。In the above, the roller device can not only keep the thickness of the material uniform, so as to facilitate the uniformity of the subsequent spraying and washing effects, but also divide the filter cloth into different working sections to avoid the liquid crossing in different working sections.
实施例三Embodiment three
本实施例是在上述实施例二的基础上进行的，与上述实施例一相同之处不予赘述。This embodiment is carried out on the basis of the above-mentioned embodiment 2, and the similarities with the above-mentioned embodiment 1 will not be repeated.
如图3所示，本实施例中，所述机身上设有6个工作段，从靠近入料装置处至靠近卸料装置处分别为工作段A71、工作段B72、工作段C73、工作段D74、工作段E75、工作段F76，每个所述工作段之间的距离相同或不同，所述真空装置也分隔为6个相互独立的腔体；所述喷淋装置位于工作段B、工作段C、工作段D、工作段E、工作段F的上方，浓酸液在工作段A处过滤、收集，滤液由工作段A处的滤液收集口排出进入真空罐，再经管道进入相应的废液存储容器；工作段B上方的喷淋装置中的喷淋水使用工作段C处的废液存储容器收集的滤液、工作段C上方的喷淋装置中的喷淋水使用工作段D处的废液存储容器收集的滤液、工作段D上方的喷淋装置中的喷淋水使用工作段E处的废液存储容器收集的滤液、工作段E上方的喷淋装置中的喷淋水使用工作段F处的废液存储容器收集的滤液、工作段F上方的喷淋装置中的喷淋水使用纯净水。As shown in Figure 3, in this embodiment, the fuselage is provided with 6 working sections, which are respectively working section A71, working section B72, working section C73, working section from near the feeding device to near the unloading device. Section D74, working section E75, working section F76, the distance between each described working section is the same or different, and the vacuum device is also divided into 6 mutually independent cavities; the spraying device is located in working section B, Above the working section C, working section D, working section E, and working section F, the concentrated acid liquid is filtered and collected at the working section A, and the filtrate is discharged from the filtrate collection port at the working section A into the vacuum tank, and then enters the corresponding pipeline through the pipeline. waste liquid storage container; the spray water in the spraying device above working section B uses the filtrate collected by the waste liquid storage container at working section C, and the spraying water in the spraying device above working section C uses working section D Use the filtrate collected by the waste liquid storage container at the working section E and the spray water in the spraying device above the working section D Use the filtrate collected by the waste liquid storage container at the working section E and the spraying water in the spraying device above the working section E Use the filtrate collected in the waste liquid storage container at the working section F, and the spray water in the spraying device above the working section F to use pure water.
基于本实施例生产高纯球形石墨用脱酸洗涤装置进行脱酸洗涤的方法，包括以下步骤：The method for deacidifying and washing with a deacidifying and washing device for producing high-purity spherical graphite based on the present embodiment may further comprise the steps:
S 1、装置运行，石墨浆料通过设置在机身一端的入料装置处供入，并均匀分布在滤布上；S 1. The device is running, and the graphite slurry is fed through the feeding device at one end of the fuselage, and evenly distributed on the filter cloth;
S2、浓酸液在工作段A处过滤、收集，滤液由滤液收集口排出进入真空装置中并收集，在工作段A处设置的超声波装置的超声波作用下，滤布上物料产生振动，使石墨粉分布更均匀，避免局部团聚形成包裹导致液体难以分离；S2. The concentrated acid liquid is filtered and collected at the working section A, and the filtrate is discharged from the filtrate collection port into the vacuum device and collected. Under the ultrasonic action of the ultrasonic device installed at the working section A, the material on the filter cloth vibrates, making the graphite The powder is more evenly distributed, avoiding partial agglomeration to form a package that makes it difficult to separate the liquid;
S3、滤布运行将石墨运送至滚轴装置处，所述滚轴装置削去石墨分布不均造成的局部突起，使物料厚度保持均匀一致，物料通过滚轴装置时受到挤压有助于水分的脱除；S3. The filter cloth runs to transport the graphite to the roller device. The roller device cuts off the local protrusions caused by the uneven distribution of graphite, so that the thickness of the material is kept uniform. When the material passes through the roller device, it is squeezed to help moisture removal of
S4、物料通过滚轴装置后移动至下一工作段中，该工作段上方的喷淋装置对物料进行喷淋，经滤布过滤后，真空装置对滤液进行收集，设置的超声波装置的超声波作用下，滤布上物料产生振动，使石墨粉分布更均匀，避免局部团聚形成包裹导致液体难以分离；S4. The material moves to the next working section after passing through the roller device. The spraying device above the working section sprays the material. After filtering through the filter cloth, the vacuum device collects the filtrate. Next, the material on the filter cloth vibrates to make the graphite powder more evenly distributed and avoid partial agglomeration to form a package that makes it difficult to separate the liquid;
S5、滤布运行将石墨运送至下一个滚轴装置处，所述滚轴装置削去石墨分布不均造成的局部突起，使物料厚度保持均匀一致，物料通过滚轴装置时受到挤压有助于水分的脱除；S5. The filter cloth runs to transport the graphite to the next roller device. The roller device cuts off the local protrusions caused by the uneven distribution of graphite, so that the thickness of the material is kept uniform. When the material passes through the roller device, it is squeezed to help in the removal of moisture;
S6、重复步骤S4-S5，直至物料在工作段B-工作段F均已完成过滤；S6. Repeat steps S4-S5 until the materials have been filtered in working section B-working section F;
S7、洗涤干净的物料在机身另一端的卸料装置中卸出。S7. The cleaned materials are unloaded from the unloading device at the other end of the fuselage.
步骤S4-S6中，所述工作段上方的喷淋装置采用的喷淋水为其后方工作段中收集的滤液，最后一个工作段上方的喷淋装置采用的喷淋水为纯净水。In steps S4-S6, the spraying water used by the spraying device above the working section is the filtrate collected in the working section behind it, and the spraying water used by the spraying device above the last working section is pure water.
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。The above description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
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