|Publication number||CN103846081 A|
|Application number||CN 201210518105|
|Publication date||11 Jun 2014|
|Filing date||6 Dec 2012|
|Priority date||6 Dec 2012|
|Also published as||CN103846081B|
|Publication number||201210518105.7, CN 103846081 A, CN 103846081A, CN 201210518105, CN-A-103846081, CN103846081 A, CN103846081A, CN201210518105, CN201210518105.7|
|Inventors||赖磊, 程祥标, 何斌, 刘强, 赵乔付|
|Export Citation||BiBTeX, EndNote, RefMan|
|Patent Citations (4), Classifications (2), Legal Events (3)|
|External Links: SIPO, Espacenet|
一种D382型树脂酸性解析工艺 One kind of acidic resin D382 analytic process
 本发明属于地浸采铀水冶处理技术领域，具体涉及D382型树脂在“高矿化、高氯根”碱法浸出条件下的解析、转型工艺。  The present invention belongs to the leaching of uranium hydrometallurgical processing technology, in particular to D382 resin in the "high salinity, high chloride" alkaline leaching conditions of analysis, transformation processes.
背景技术 酸法地浸技术在伊犁铀矿山取得成功并在全国迅速发展，但在地质条件更为复杂的某矿山只能用弱试剂中性浸出工艺，同时此矿山矿石品位低，浸出液铀浓度低，浸出液的“高矿化度、高氯离子”使得大部分树脂基本不吸附铀，在化冶院合作下开发出了D382型树月旨，采取此型号树脂浸出液后处理工艺流程能够适应于该矿床“高矿化度、高氯离子”含量的浸出液处理，并能够满足于“低浓度、大流量”的浸出液工艺条件。  Acid leaching technology to obtain success in the Ili and the rapid development of uranium mines in the country, but in a more complex geological conditions, mine only weak neutral leaching reagents, while the low-grade ore mining, leachate low uranium leaching solution "high salinity, high chloride" is not making the most basic resin adsorption of uranium, Metallurgical Academy in cooperation to develop a type of tree months D382 aims to take after this model resin leachate treatment process can leachate treatment adapted to the deposit of "high salinity, high chloride" content, and the ability to meet the "low density, high flow" leachate process conditions. 但工业实验初期树脂处理需分两步进行，氯化钠加碳酸氯铵进行碱性解析，然后再用工业盐酸进行转型，此工艺流程过多，操作麻烦，工作量大，原材料的消耗大，操作过程氨气排放不利工人身心健康。 But initial experiments resin processing industry needs two steps, sodium carbonate, ammonium chloride were added to the basic resolution, and then use the transformation of industrial hydrochloric acid, this process too, operational problems, heavy workload, raw material consumption, ammonia emissions during operation adverse physical and mental health workers. 因此，极需开发一种废气排放减少、作业易操作且更环保的D382型树脂酸性解析工艺。 Therefore, the need to develop a highly reducing emissions, the job is easy to operate and more environmentally friendly resin D382 acidic analytical processes.
 本发明的目的是克服现有技术的缺陷，提供一种D382型树脂在“高矿化、高氯根”碱法浸出条件下的操作简便且环保的解析、转型工艺。  The object of the present invention to overcome the deficiencies of the prior art, to provide a simple type resin D382 at "high salinity, high chloride" Alkaline Leaching conditions of operation and environmental analysis, the transformation process.
 为了实现上述目的，本发明的技术方案为，一种D382型树脂酸性解析工艺，包含以下步骤:  To achieve the above object, the present invention is directed to a D382-type resin acid analytical process, comprising the steps of:
 步骤1，D382型树脂吸附饱和后，经反洗工序将吸附于树脂颗粒间隙中的泥沙等杂质清理，后用0.2MPa压强的压缩空气将树脂颗粒间隙中的液体排干备用；  Step 1, the D382 resin adsorption saturation, the backwash process will clean up the impurities adsorbed on the resin particles such as silt gap after use of compressed air pressure 0.2MPa resin particles in the liquid drained gap spare;
 步骤2，将合格液、工业盐酸按照体积比14~16:3的比例配制成酸化液，配置酸化液的体积须满足将包含D382型树脂的吸附塔完全充满后，还有Im3的余量；然后将其中60%的酸化液送到吸附塔内，对经步骤I处理后的D382型树脂进行浸泡，浸泡时间为6~8小时；  Step 2, the passing liquid, industrial hydrochloric acid in a volume ratio of 14 ~ 16: 3 ratio formulated as acidizing fluids, acidizing fluids configuration shall meet volume containing the adsorber resin D382 completely filled, there was always the Im3 balance; then 60% of the acidified solution to the adsorption column, after the step of processing the D382 type I resin soaking, the soaking time of 6-8 hours;
 步骤3，将吸附塔内和吸附塔外的的酸化液进行循环，循环方式采用下进液，上出液的方式；循环6~8小时后监测循环液pH，当进液与出液pH值达到一致且≥1.5时停止循环；若pH值未达标，补加0.5m3工业盐酸，继续循环，直到进液与出液pH值达到一致且(1.5时为止;  Step 3, the adsorption tower in the adsorption tower and the outside of the acidizing fluid is circulated down into the liquid using a circular manner, on the way out of the liquid; pH monitoring fluid circulating loop 6 to 8 hours later, when the feed solution and the pH value ≥1.5 achieve consistent and stop the cycle; if the pH value is not reached, additional 0.5m3 industrial hydrochloric acid, the cycle continues until the inlet and the pH value and achieve the same (up 1.5;
 步骤4，完成步骤3后进入解析工序，解析工序选用解析剂为3~4g/L的盐酸溶液，采用三塔串联解析，解析方式采用上进液、下出液，吸附塔内解析液的线速度为0.8~  Step 4, after completing step 3 into the analytical process, analytical selection process to resolve agent hydrochloric acid solution for 3 ~ 4g / L, using the three towers series analysis, analytical methods were adopted to make progress under the liquid adsorption tower analytical solution The linear velocity of 0.8 to
1.0m/h ;当解析出液流比达到2左右时停止进解析剂，获得解析合格液；然后向三塔中的首塔进0.2MP的压缩空气，继续解析，出液至酸化液储槽，加工业盐酸配制成酸化液后用于其他吸附塔的解析；进压缩空气将首塔压干后结束解析工序，转入步骤5 ； 1.0m / h; when parsing a flow ratio of around 2 stop into parsing agent to obtain qualified analytical solution; 0.2MP compressed air and then into the first tower to the three towers, continue to resolve, a solution to the acidified liquid storage tank plus industrial hydrochloric acid formulated into liquid after acidification for resolving other adsorption tower; compressed air into the tower after the end of the first pressed dry analytical process, go to Step 5;
 步骤5，向首塔注入清水洗涤，线速度为2m/h，直至出液铀浓度小于lmg/L且pH值大于4.0方可停止； 步骤6，将步骤4得到的解析合格液进行中性沉淀:往解析合格液中边加入NaOH边搅拌，搅拌均匀后测量PH值，直至pH值为7.0~8.0时，停止加入NaOH和搅拌，进行沉淀；沉淀12小时后，排出上清液，再加同样体积的解析合格液，重复本步骤中的中性沉淀步骤，直到沉淀次数达到70次后，进行板框压滤操作获得产品。  Step 5, the first column was washed with water injection, a linear velocity of 2m / h, until the liquid uranium concentration of less than lmg / L and a pH greater than 4.0 before the stop;  Step 6, Step 4 was resolved Qualified neutral liquid precipitation: qualified to resolve while adding NaOH solution while stirring, measuring PH value Stir until the pH value of 7.0 to 8.0, stop adding NaOH and stirred precipitation; precipitation 12 hours after discharge on serum, together with the same volume of liquid analytical qualified, repeat this step neutral precipitation step, until the precipitate reaches 70 times the number, frame filter press operation performed to obtain product.
 所述步骤3中，当进液与出液pH值达到一致且≤1.3时停止循环。  The step 3, consistent, and when you stop the cycle when ≤1.3 into the liquid with a pH value reached.
 所述步骤4中，解析工序选用解析剂为3.5g/L的盐酸溶液。  In the step 4, the choice of analytical analysis step hydrochloric acid solution agent is 3.5g / L of.
 所述步骤6中，合格液沉淀完全后，加入1.5倍浆体体积清水进行清水沉淀，排完上清液后，再进板框压滤操作获得产品。  The step 6, after passing the liquid precipitation completely, 1.5 times the volume of water to make a slurry of water precipitation, the supernatant was drained, and then into the frame filter press operation to obtain the product.
 本发明的进步之处在于简化了解析工艺，降低了解析流比，提高了合格液铀浓度，去除了工艺盐和碳酸氢铵的消耗；与碱性解析工艺相比，降低了生产成本，减轻了员工的工作强度，除去了氨气的排放，操作流程更加简单且环保。  at the progress of the present invention is to simplify the analytical process and reduce the parsing flow ratio, improve the passing liquid uranium concentration, in addition to the consumption of process salts and ammonium bicarbonate; compared with the basic analytical process, reducing production costs, reduce the intensity of the work of employees, to remove the ammonia emissions, operational processes more simple and environmentally friendly.
具体实施方式 DETAILED DESCRIPTION
 下面结合实施例对本发明进行进一步描述。  below with reference to embodiments of the present invention will be further described.
 实施装置  The device
 一种D382型树脂酸性解析工艺，借助于以下已有的装置实施:  A D382 resin acid parsing process, by means of the following conventional apparatus embodiment:
 a.吸附塔:吸附塔为直径2.5m铁罐，总高为7.5m，有效高度为6m，内衬PO，部件包括:塔底接口，DN200法兰，为液体出液口；塔顶接口，DN25，安装压力表用；塔顶接口，DN500法兰，为原液进液口；塔顶接口，DN40，与压缩空气管道相连；压缩空气管道为DN50铁管，其余连接管道均为PPR管材，尺寸和法兰尺寸对应。 .  a adsorption tower: 2.5m diameter cans adsorption tower, with a total height of 7.5m, the effective height of 6m, lined PO, components include: bottom interface, DN200 flange, liquid liquid outlet; tower top interface, DN25, install pressure gauges used; overhead interface, DN500 flange for liquid inlet port; overhead interface, DN40, connected with the air duct; compressed air piping for DN50 iron pipes, connecting pipes are PPR rest corresponding pipe size and flange dimensions.
 b.解析剂储槽:直径2.5m铁罐，高度为2m，内衬PO，部件包:塔顶接口，DN40法兰，由DN40铁管与清水管道连接；塔顶排气口，40cm*40cm ;塔底接口，DN40法兰，解析剂出液口，由DN40的PPR管子与解析剂输送泵连接。 .  b parsing agent reservoir: 2.5m diameter cans, a height of 2m, lined PO, part package: overhead interface, DN40 flange connection DN40 iron pipe with water by pipeline; overhead vent, 40cm * 40cm; bottom interface, DN40 flange, parsing agent liquid outlet, the PPR pipes from DN40 pump connection with the analytical agent.
 c.酸化液储槽:直径2.5m铁罐，高4m，内衬PO，部件包括:塔顶接口，DN40法兰，由DN40铁管与清水管道连接；塔顶接口，DN40法兰，由DN40PPR管道接盐酸管道；塔顶排气口，DN50 ;塔顶接口，DN80法兰，酸化循环回水，由DN80PPR管道连接；塔底接口，DN80法兰，酸化液出液用，接DN80PPR管道。  c acidizing fluid reservoir: 2.5m diameter cans, high-4m, lined PO, components include: overhead interface, DN40 flange connection DN40 iron pipe with water by pipeline; tower interface, DN40 flange by DN40PPR pipeline connection hydrochloric pipeline; overhead vent, DN50; tower interface, DN80 flange, acidification circulating backwater, connected by DN80PPR pipeline; bottom interface, DN80 flange, acidified solution with a solution, then DN80PPR pipe.
 d.原液池:原液池为长25m，宽20m，高3.5m水泥槽，部件包括:原液进液口，长40cm,宽40cm ;排气口，长40cm，宽40cm ;排气口，长40cm，宽40cm ;原液出液口，DN200法兰，由DN200铁管和进塔泵对接。 .  d liquid pool: liquid pool length 25m, width 20m, height 3.5m cement tanks, components include: liquid fluid intake, long 40cm, width 40cm; vent length 40cm, width 40cm; vent length 40cm, width 40cm; dope liquid outlet, DN200 flange, DN200 iron pipe from the pump into the tower and docking.
 e.母液池:母液池长6m，宽6m，高2m铁槽，部件包括:DN40铁管，拍母液池中清液用。  e liquor pool: liquor pool length 6m, width 6m, 2m high iron trough, components include: DN40 iron pipe, shoot pool with the supernatant liquor.
 f.沉淀槽:直径1.5m,高3.3m铁罐，内衬PO，部件包括:罐顶接口，DN40法兰，由DN40PPR管道与合格液管道连接；罐顶接口，DN40法兰，由DN40PPR管道与清水管道连接；罐顶接口，DN40法兰，由DN40PPR管道与板块回水管道连接；罐顶口，长40cm，宽40cm，沉淀加片碱用；罐底接口，DN40法兰，打板框出浆口，由DN40PPR管道连接。  f the sedimentation tank: diameter of 1.5m, 3.3m tall cans lined PO, components include: tank top interface, DN40 flange, connected by pipeline with qualified DN40PPR liquid pipeline; tank top interface, DN40 flange. connected by pipes and water pipes DN40PPR; tank top interface, DN40 flanges, pipes and plates connected by DN40PPR return pipe; tank top opening, length 40cm, width 40cm, precipitated by adding caustic soda; tank bottom interface, DN40 flange, beat the pulp out of the mouth frame, connected by DN40PPR pipe.
 实施步骤 Implementation steps 
 步骤1，D382型树脂吸附饱和后，经反洗工序将吸附于树脂颗粒间隙中的泥沙等杂质清理，后用0.2MPa压强的压缩空气将树脂颗粒间隙中的液体排干备用； 步骤2，某铀矿山采用15m3铀浓度小于5g/L的合格液中加入3m3工业盐酸的比例配制成吸附塔容积一致的酸化液，由酸化液输送泵将60%的酸化液输送至吸附塔内对树脂进行浸泡；合格液指的是地浸技术中饱和树脂经解析剂解析后的含铀液体，工业盐酸为质量百分比为31%有的HCl溶液，浸泡时间8小时；；  Step 1, the D382 resin adsorption saturation, the backwash process will clean up the impurities adsorbed on the resin particles such as silt gap after use of compressed air pressure 0.2MPa resin particles in the liquid drained gap spare;  Step 2, a uranium mine uranium using 15m3 less than 5g / L qualified industrial hydrochloric acid was added 3m3 proportion formulated into a consistent volume of adsorption column acidizing fluid, transmission fluid pump by acidification to 60% of the acidified liquid delivered to resin adsorption tower soaking; qualified liquid immersion technique refers to saturated liquid resin containing uranium, industrial hydrochloric acid as a percentage of the quality of 31% HCl solution and some agents parsed parsed, soak 8 hours ;;
 步骤3，将吸附塔内和吸附塔外的酸化液进行循环，循环方式采用下进液，上出液的方式；循环6~8小时后监测循环液pH，当进液与出液pH值达到一致且≤优选1.3时停止循环；若PH值未达标，补加0.5m3工业盐酸，继续循环，直到进液与出液pH值达到一致且(1.3时为止;  Step 3, the adsorption tower and the acidified solution is circulated outside the adsorption tower, a circular manner using lower into the liquid, the liquid on the way; pH monitoring fluid circulating loop 6 to 8 hours later, when the liquid inlet and the liquid pH value reached consensus and stop cycle ≤ 1.3 is preferable; if PH value is not standard, additional 0.5m3 industrial hydrochloric acid, the cycle continues until the inlet and the fluid pH to a consistent and (until 1.3;
 步骤4,完成步骤3后进入解析工序,解析工序选用解析剂为3.5g/L的盐酸溶液，采用三塔串联解析，解析方式采用上进液、下出液，吸附塔内解析液的线速度为0.8~  Step 4, after completing step 3 into the analytical process, analytical hydrochloric acid solution selection process to resolve agent 3.5g / L, the use of three towers series analysis, analytical methods were adopted to make progress under the liquid adsorption tower analytic solution linear velocity of 0.8 to
1.0m/h ;当电子流量计测得的解析出液流比达到2左右时停止进解析剂，获得解析合格液；然后开启空压机，向三塔中的首塔进0.2MP的压缩空气，继续解析，出液至酸化液储槽，加工业盐酸配制成酸化液后用于其他吸附塔的解析，进压缩空气将首塔压干后结束解析工序，转入步骤5的漂洗工序；本实施例中，首塔压干时首塔解析液铀浓度小于800mg/L，解析前的D382型树脂是饱和树脂，经步骤4解析后成为贫树脂，首塔贫树脂残余铀容量小于Ig/L ； 1.0m / h; electronic meter when measured parse out the flow ratio of around 2 stop into parsing agent to obtain qualified analytical solution; then, turn on the air compressor, the three towers in the first column of compressed air into the 0.2MP continuing resolution, a solution to the acidified liquid storage tank, the preparation of hydrochloric acid into the industry after acidification was used to resolve other adsorption tower into the air after the first tower pressed dry end analytical process, go to Step 5 of the rinsing step; this embodiment, the first column when the first column pressure dry analytical liquid uranium concentration is less than 800mg / L, D382-type resin resolved before the resin is saturated, after step 4 resolves become depleted resin, the first resin column depleted uranium residue capacity is less than Ig / L ;
 步骤5，向首塔注入清水洗涤，控制流量为10m3/h，直至出液铀浓度小于lmg/L且PH值大于4.0方可停止，以达到回收树脂上残余铀和提高吸附塔内体系pH值的目的；  Step 5, the first tower into washing water, to control the flow of 10m3 / h, until the liquid uranium concentrations less than lmg / L and the PH value greater than 4.0 before the stop, in order to achieve the recovery of uranium and increase the residual resin adsorption tower The purpose of the pH value;
 步骤6，将步骤4得到的解析合格液进行中性沉淀:将解析合格液用泵打入沉淀槽中，边搅拌边加入片碱，合格液距沉淀槽顶IOcm左右停止进液，搅拌5分钟后调节pH值至  Step 6, Step 4 will parse qualified solution was subjected to neutral precipitation: qualified solution will resolve into the sedimentation tank with pump, while stirring, caustic soda, liquid from the settling tank top qualified IOcm about stopping into the liquid, adjusting the pH after stirring for 5 minutes to
7.0~8.0，若pH不够，补加适量片碱继续搅拌，直到pH达标为止，停止搅拌进行沉淀；12小时后排上清液去母液池，然后再加合格液继续重复前面的步骤。 7.0 to 8.0, if the pH is not enough to make up plus the amount of caustic soda and continue stirring until the pH compliance date, stop stirring precipitation; 12 hours to go back supernatant liquor tank, then add the liquid passing continue to repeat the previous step. 当沉淀次数达到70次以上时方可进行板框压滤操作，降低产品杂质含量，提高产品品位，合格液沉淀完全后，向沉淀槽中加入约1.5倍浆体体积清水进行清水沉淀，排完上清液后方可进行打板框工序获得 When the number has risen to 70 times more precipitation can be carried out when the frame filter press operations, reduce product impurities, improve product quality, fully qualified solution after precipitation, the precipitation tank by adding about 1.5 times the volume of water to make a slurry of water precipitation, drained before they are allowed to play the supernatant obtained after step frame
女口 Female mouth
广叩ο Canton knock ο
 实施结果:本发明与碱性解析合格液沉淀所得产品的参数对比和经济指标对比见表1和表2:  The result: This invention relates to an alkaline liquid analytical parameters compared qualified and economic indicators precipitation resulting product compared in Table 1 and Table 2:
 表1:两种产品参数对比  Table 1: Comparison of both products parameters
 表2两种工艺经济指标  Table 2. The two processes of economic indicators
 从表1可以看出，与碱性解析合格液沉淀所得产品相比具有一定优势，产品铀品位可提高约7%，，氯离子含量降低约1%。  As can be seen from Table 1, compared with the alkaline solution was precipitated resultant analytical qualified products have certain advantages, uranium product quality can be improved by about 7% ,, chlorine ion content reduced by about 1%.
 从表2可以看出，通过此工艺将碱性解析-酸性转型两步工艺简化为一步完成，解析流比由3左右降至2.0左右，合格液铀浓度由8g/L左右提高到12g/L左右，除去了工艺盐和碳酸氢铵的消耗，与碱性解析工艺相比生产每吨铀可降低生产成本约1.4万元，同时减轻了员工的工作强度，除去了氨气的排放，操作流程更加简单且环保。  As can be seen from Table 2, through this process will be the basic parsing - a two-step process to simplify the transition to acidic step, analytical flow ratio is about to fall to about 2.0 by 3 qualified liquid uranium concentrations by about 8g / L increased to about 12g / L, remove the salt and bicarbonate consumption process, compared with the basic analytical process to produce a tonne of uranium can reduce the production cost of about 1.4 million, while reducing the intensity of the work of employees, to remove the ammonia emissions , operational processes more simple and environmentally friendly.
 上面对本发明的实施例作了详细说明，上述实施方式仅为本发明的最优实施例，但是本发明并不限于上述实施例，在本领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下作出各种变化。 Faced with embodiments of the present invention have been  described in detail on the above embodiments are merely preferred embodiments of the invention, but the present invention is not limited to the above embodiments, the ordinary skill in the art possess knowledge of, various changes may be made without departing from the spirit of the present invention is the premise.
|Cited Patent||Filing date||Publication date||Applicant||Title|
|CN101195862A *||20 Dec 2007||11 Jun 2008||金川集团有限公司||Method for purifying and cadmium removing from nickel and cobalt solution|
|CN101224436A *||25 Sep 2007||23 Jul 2008||张剑秋;张复兴||Ion exchange resin regeneration method|
|CN102219258A *||14 Apr 2010||19 Oct 2011||湖南荣宏钼业材料股份有限公司||Method for extracting molybdenum from waste materials in ammonium molybdate production field|
|US4242097 *||5 Mar 1979||30 Dec 1980||Dionex Corporation||Method and apparatus for quantitative analysis of weakly ionized anions or cations|
|11 Jun 2014||C06||Publication|
|9 Jul 2014||C10||Entry into substantive examination|
|29 Jun 2016||C14||Grant of patent or utility model|