WO2018148869A1 - Leaching solution for waste incineration fly ash chelate and preparation and application methods therefor - Google Patents

Leaching solution for waste incineration fly ash chelate and preparation and application methods therefor Download PDF

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WO2018148869A1
WO2018148869A1 PCT/CN2017/073538 CN2017073538W WO2018148869A1 WO 2018148869 A1 WO2018148869 A1 WO 2018148869A1 CN 2017073538 W CN2017073538 W CN 2017073538W WO 2018148869 A1 WO2018148869 A1 WO 2018148869A1
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deionized water
beaker
extract
fly ash
sulfuric acid
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刘红
赵晓峰
谭巍
叶宇洋
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深圳市能源环保有限公司
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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Abstract

Disclosed are a leaching solution for a waste incineration fly ash chelate and preparation and application methods therefor. The leaching solution is composed of components such as sulfuric acid, glacial acetic acid, boric acid and deionized water. The preparation method therefor comprises the following steps: step one, 0.2-1.2 mg of boric acid is weighed and diluted and dissolved with 200 ml of deionized water for later use; step two, 0.5-1.5 ml of glacial acetic acid with a concentration of 99.5% is transferred and then diluted with 200 ml of deionized water for later use; step three, 1580-1590 ml of deionized water is measured with a measuring cylinder and poured into a beaker, and then, 10-20 ml of concentrated sulfuric acid with a concentration of 98% is measured with a measuring cylinder, the concentrated sulfuric acid is injected into the beaker and stirred continuously with a glass rod and cooled for later use; and step four, the solutions formulated in steps 2 and 3 are slowly added into a beaker of step 1 and stirred until uniform, wherein after cooling, the solution is transferred into a volumetric flask for later use. At the same time, also provided is a method for leaching the toxicity of a fly ash chelate by using the above leaching solution, which method can improve the efficiency of detecting large quantities of samples every day and provide a pre-treatment method for online monitoring technologies, thus making online monitoring possible.

Description

一种垃圾焚烧飞灰螯合物浸提液及其制备应用方法Waste incineration fly ash chelate extract liquid and preparation application method thereof 技术领域Technical field
本发明涉及一种垃圾焚烧厂固体废物浸提剂,尤其是涉及一种垃圾焚烧飞灰螯合物浸提液及其制备应用方法。The invention relates to a waste incineration plant solid waste extracting agent, in particular to a garbage incineration fly ash chelate extracting liquid and a preparation method thereof.
背景技术Background technique
现有垃圾焚烧厂一般采用无机或有机药剂对飞灰进行稳定化处理,处理后的飞灰螯合物需每天进行多个样品的浸出毒性检测,达《生活垃圾填埋污染控制标准》(GB16889-2008)要求后方可送入生活垃圾填埋厂填埋。GB16889-2008规定飞灰螯合物浸出毒性应采用醋酸缓冲溶液法(HJ/T 300-2007)方法进行预处理后上机检测,但该预处理方法单个样品需耗时18~20h,由于预处理时间长,因此不具备在线监测条件。Existing waste incineration plants generally use inorganic or organic agents to stabilize fly ash. The treated fly ash chelates need to be tested for leaching toxicity of multiple samples every day, reaching the “Standard for Pollution Control of Domestic Waste Landfill” (GB16889) -2008) Requirement can be sent to the landfill of the domestic waste landfill. GB16889-2008 stipulates that the leaching toxicity of fly ash chelate should be pretreated by acetic acid buffer solution (HJ/T 300-2007), but the pretreatment method takes 18-20 hours for a single sample. The processing time is long and therefore there is no online monitoring condition.
发明内容Summary of the invention
为了解决现有技术存在的问题,本发明提供一种快速、准确的预处理方法,提高每天大批量样品检测效率,为在线监测技术提供前置预处理方法,使在线监测成为可能。In order to solve the problems existing in the prior art, the present invention provides a fast and accurate pretreatment method, which improves the detection efficiency of large-scale samples per day, and provides a pre-processing method for online monitoring technology, thereby making online monitoring possible.
本发明解决问题所采用的技术方案是,一种垃圾焚烧飞灰螯合物浸提液,其特征是,由硫酸、冰乙酸、硼酸及去离子水等成分组成,以摩尔比计算,其中硫酸、冰乙酸、硼酸分别与去离子水的摩尔比为:The technical solution adopted by the present invention is a garbage incineration fly ash chelate extract, which is characterized in that it is composed of sulfuric acid, glacial acetic acid, boric acid and deionized water, and is calculated by a molar ratio of sulfuric acid. The molar ratio of glacial acetic acid and boric acid to deionized water is:
硫酸:去离子水=0.138:1Sulfuric acid: deionized water = 0.138:1
冰乙酸:去离子水=0.013:1Glacial acetic acid: deionized water = 0.113:1
硼酸:去离子=0.012:1Boric acid: deionized = 0.012:1
本发明解决问题所采用的技术方案是,一种垃圾焚烧飞灰螯合物浸提液的制备方法,其特征是,包括如下步骤:The technical solution adopted by the present invention for solving the problem is a method for preparing a waste incineration fly ash chelate extract, which comprises the following steps:
第1步,称取硼酸0.2-1.2mg,然后用200ml去离子水稀释溶解,备用。In the first step, 0.2-1.2 mg of boric acid is weighed, and then diluted and dissolved in 200 ml of deionized water for use.
第2步,移取冰乙酸0.5-1.5ml(浓度99.5%),然后用200ml去离子水稀释,备用。In the second step, 0.5-1.5 ml of glacial acetic acid (99.5% concentration) was removed, and then diluted with 200 ml of deionized water for use.
第3步,量筒量取1580-1590ml去离子水,倒入烧杯中,再用量筒量取10-20ml浓硫酸(浓度98%),将浓硫酸注入烧杯中,并用玻璃棒不断搅拌,冷却后备用;In the third step, the measuring cylinder is taken with 1580-1590ml of deionized water, poured into a beaker, and then the measuring cylinder is used to measure 10-20ml of concentrated sulfuric acid (concentration 98%), the concentrated sulfuric acid is injected into the beaker, and the glass rod is continuously stirred and cooled. use;
第4步,将步骤2、3配制好的溶液缓慢加入步骤1的烧杯中搅匀,冷却后移入容量瓶中,备用。In the fourth step, the solutions prepared in steps 2 and 3 are slowly added to the beaker of step 1 and stirred, cooled, and transferred to a volumetric flask for use.
一种飞灰螯合物毒性浸提方法,其特征是,包括如下步骤:A fly ash chelate toxic extraction method, characterized in that the method comprises the following steps:
第1步,将待检样品经人工破碎并过9.5mm的筛网(涂Teflon的筛网),取0.5-1g筛下物至快速水分检测仪进行检测,确定其含水率,In the first step, the sample to be inspected is manually crushed and passed through a 9.5 mm sieve (Teflon-coated sieve), and 0.5-1 g of the sieve is taken to a rapid moisture detector for determination to determine the water content.
第2步,取100g样品至聚四氟乙烯(PTFE)烧杯中,根据步骤1测得的样品含水率计算出样品中固相、液相含量,然后以固体重量单位为kg、液体体积单位为L,按照固液比1:20比例计算出上述浸提液 的体积,量取浸提液并将浸提液加入到烧杯中,人工快速搅拌5min;In the second step, 100g sample is taken into a polytetrafluoroethylene (PTFE) beaker, and the solid phase and liquid phase content in the sample are calculated according to the moisture content of the sample measured in step 1, and then the solid weight unit is kg, and the liquid volume unit is L, the above extract is calculated according to the ratio of solid to liquid ratio of 1:20 The volume, the extract is taken and the extract is added to the beaker and stirred rapidly for 5 minutes by hand;
第3步,将步骤2的烧杯置于恒温磁力搅拌器上,设置温度为40~70℃,转速为50~130r/min,搅拌时间为1~2h。In the third step, the beaker of step 2 is placed on a constant temperature magnetic stirrer, the temperature is set to 40 to 70 ° C, the rotation speed is 50 to 130 r / min, and the stirring time is 1 to 2 h.
第4步,通过0.45μm膜过滤后获得浸提液。In the fourth step, the extract was obtained by filtration through a 0.45 μm membrane.
本发明的有益效果是:采用一种快速浸提剂及特殊浸出方法对飞灰螯合物进行预处理,有效缩短反应时间,预处理时间由原18~20h缩短至1~2h,浸提效果与醋酸缓冲溶液法(HJ/T 300-2007)方法相同,特别适合大批量飞灰螯合物检测工作,为在线监测飞灰螯合物浸出毒性创造了条件。The invention has the beneficial effects that the fly ash chelate is pretreated by a rapid leaching agent and a special leaching method, and the reaction time is shortened effectively, and the pretreatment time is shortened from the original 18-20 h to 1-2 h, and the leaching effect is obtained. It is the same as the acetic acid buffer solution method (HJ/T 300-2007), and is especially suitable for the detection of large quantities of fly ash chelate, which creates conditions for online monitoring of leaching toxicity of fly ash chelate.
具体实施方式detailed description
实施例1Example 1
一种垃圾焚烧飞灰螯合物浸提液的制备方法,其特征是,包括如下步骤:A method for preparing a waste incineration fly ash chelate extract, characterized in that the method comprises the following steps:
第1步,称取硼酸0.2mg,然后用200ml去离子水稀释溶解,备用。In the first step, 0.2 mg of boric acid was weighed and then diluted with 200 ml of deionized water to be used.
第2步,移取冰乙酸0.5ml(浓度99.5%),然后用200ml去离子水稀释,备用。In the second step, 0.5 ml of glacial acetic acid (99.5% concentration) was removed, and then diluted with 200 ml of deionized water for use.
第3步,量筒量取1580ml去离子水,倒入烧杯中,再用量筒量取10ml浓硫酸(浓度98%),将浓硫酸注入烧杯中,并用玻璃棒不断搅拌,冷却后备用;In the third step, the measuring cylinder is taken with 1580 ml of deionized water, poured into a beaker, and then 10 ml of concentrated sulfuric acid (concentration 98%) is taken in a measuring cylinder, concentrated sulfuric acid is poured into the beaker, and continuously stirred with a glass rod, and cooled for use;
第4步,分别将步骤2、3配制好的溶液缓慢加入步骤1的烧杯中搅匀,冷却后移入容量瓶中,备用。In the fourth step, the solutions prepared in steps 2 and 3 are slowly added to the beaker of step 1 and stirred, cooled, and transferred to a volumetric flask for use.
实施例2Example 2
一种垃圾焚烧飞灰螯合物浸提液的制备方法,其特征是,包括如下步骤:A method for preparing a waste incineration fly ash chelate extract, characterized in that the method comprises the following steps:
第1步,称取硼酸0.8mg,然后用200ml去离子水稀释溶解,备用。In the first step, 0.8 mg of boric acid was weighed and then diluted and dissolved in 200 ml of deionized water for use.
第2步,移取冰乙酸1.0ml(浓度99.5%),然后用200ml去离子水稀释,备用。In the second step, 1.0 ml of glacial acetic acid (99.5% concentration) was removed, and then diluted with 200 ml of deionized water for use.
第3步,量筒量取1585ml去离子水,倒入烧杯中,再用量筒量取15ml浓硫酸(浓度98%),将浓硫酸注入烧杯中,并用玻璃棒不断搅拌,冷却后备用;In the third step, the measuring cylinder is taken with 1585 ml of deionized water, poured into a beaker, and then 15 ml of concentrated sulfuric acid (concentration 98%) is taken in a measuring cylinder, concentrated sulfuric acid is poured into the beaker, and continuously stirred with a glass rod, and cooled for use;
第4步,分别将步骤2、3配制好的溶液缓慢加入步骤1的烧杯中搅匀,冷却后移入容量瓶中,备用。In the fourth step, the solutions prepared in steps 2 and 3 are slowly added to the beaker of step 1 and stirred, cooled, and transferred to a volumetric flask for use.
实施例3Example 3
一种垃圾焚烧飞灰螯合物浸提液的制备方法,其特征是,包括如下步骤:A method for preparing a waste incineration fly ash chelate extract, characterized in that the method comprises the following steps:
第1步,称取硼酸1.2mg,然后用200ml去离子水稀释溶解,备用。In the first step, 1.2 mg of boric acid was weighed and then diluted and dissolved in 200 ml of deionized water for use.
第2步,移取冰乙酸1.5ml(浓度99.5%),然后用200ml去离子水稀释,备用。In the second step, 1.5 ml of glacial acetic acid (99.5% concentration) was removed, and then diluted with 200 ml of deionized water for use.
第3步,量筒量取1590ml去离子水,倒入烧杯中,再用量筒量取20ml浓硫酸(浓度98%),将浓硫酸注入烧杯中,并用玻璃棒不断搅拌,冷却后备用;In the third step, the measuring cylinder is taken with 1590 ml of deionized water, poured into a beaker, and then 20 ml of concentrated sulfuric acid (concentration 98%) is taken in a measuring cylinder, concentrated sulfuric acid is poured into the beaker, and continuously stirred with a glass rod, and cooled for use;
第4步,将步骤2、3配制好的溶液缓慢加入步骤1的烧杯中搅匀,冷却后移入容量瓶中,备用。In the fourth step, the solutions prepared in steps 2 and 3 are slowly added to the beaker of step 1 and stirred, cooled, and transferred to a volumetric flask for use.
实施例4 Example 4
一种飞灰螯合物毒性浸提方法,其特征是,包括如下步骤:A fly ash chelate toxic extraction method, characterized in that the method comprises the following steps:
第1步,将待检样品经人工破碎并过9.5mm的筛网(涂Teflon的筛网),取0.5-1g筛下物至快速水分检测仪进行检测,确定其含水率,In the first step, the sample to be inspected is manually crushed and passed through a 9.5 mm sieve (Teflon-coated sieve), and 0.5-1 g of the sieve is taken to a rapid moisture detector for determination to determine the water content.
第2步,取100g样品至聚四氟乙烯(PTFE)烧杯中,根据步骤1测得的样品含水率计算出样品中固相、液相含量,然后以固体重量单位为kg、液体体积单位为L,按照固液比1:20比例计算出上述浸提液的体积,量取浸提液并将浸提液加入到烧杯中,人工快速搅拌5min;In the second step, 100g sample is taken into a polytetrafluoroethylene (PTFE) beaker, and the solid phase and liquid phase content in the sample are calculated according to the moisture content of the sample measured in step 1, and then the solid weight unit is kg, and the liquid volume unit is L, according to the ratio of solid to liquid ratio of 1:20 to calculate the volume of the above extract, the amount of extract and extract the extract into the beaker, artificial rapid stirring for 5min;
第3步,将步骤2的烧杯置于恒温磁力搅拌器上,设置温度为40~70℃,转速为50~130r/min,搅拌时间为1~2h。In the third step, the beaker of step 2 is placed on a constant temperature magnetic stirrer, the temperature is set to 40 to 70 ° C, the rotation speed is 50 to 130 r / min, and the stirring time is 1 to 2 h.
第4步,通过0.45μm膜过滤后获得浸提液。 In the fourth step, the extract was obtained by filtration through a 0.45 μm membrane.

Claims (3)

  1. 一种垃圾焚烧飞灰螯合物浸提液,其特征是,由硫酸、冰乙酸、硼酸及去离子水等成分组成,以摩尔比计算,其中硫酸、冰乙酸、硼酸分别与去离子水的摩尔比为:A waste incineration fly ash chelate extract characterized by being composed of sulfuric acid, glacial acetic acid, boric acid and deionized water, and calculated by molar ratio, wherein sulfuric acid, glacial acetic acid, boric acid and deionized water respectively The molar ratio is:
    硫酸:去离子水=0.138:1Sulfuric acid: deionized water = 0.138:1
    冰乙酸:去离子水=0.013:1Glacial acetic acid: deionized water = 0.113:1
    硼酸:去离子=0.012:1Boric acid: deionized = 0.012:1
  2. 一种垃圾焚烧飞灰螯合物浸提液的制备方法,其特征是,包括如下步骤:A method for preparing a waste incineration fly ash chelate extract, characterized in that the method comprises the following steps:
    第1步,称取硼酸0.2-1.2mg,然后用200ml去离子水稀释溶解,备用;In the first step, weigh 0.2-1.2mg of boric acid, then dilute it with 200ml of deionized water, and set aside;
    第2步,移取浓度99.5%冰乙酸0.5-1.5ml,然后用200ml去离子水稀释,备用;In the second step, the concentration of 99.5% glacial acetic acid 0.5-1.5ml is removed, and then diluted with 200ml of deionized water for use;
    第3步,量筒量取1580-1590ml去离子水,倒入烧杯中,再用量筒量取浓度98%浓硫酸10-20ml,将浓硫酸注入烧杯中,并用玻璃棒不断搅拌,冷却后备用;In the third step, the measuring cylinder is taken with 1580-1590 ml of deionized water, poured into a beaker, and then the measuring cylinder is used to measure the concentration of 98% concentrated sulfuric acid 10-20 ml, and the concentrated sulfuric acid is poured into the beaker, and continuously stirred with a glass rod, and cooled for use;
    第4步,将步骤2、3配制好的溶液缓慢加入步骤1的烧杯中搅匀,冷却后移入容量瓶中,备用。In the fourth step, the solutions prepared in steps 2 and 3 are slowly added to the beaker of step 1 and stirred, cooled, and transferred to a volumetric flask for use.
  3. 一种利用权利要求1所述浸提液进行飞灰螯合物毒性浸提的方法,其特征是,包括如下步骤:A method for toxic leaching of fly ash chelates by using the extract of claim 1 , comprising the steps of:
    第1步,将待检样品经人工破碎并过9.5mm的筛网,取0.5-1g筛下物至快速水分检测仪进行检测,确定其含水率;In the first step, the sample to be inspected is manually crushed and passed through a sieve of 9.5 mm, and 0.5-1 g of the sieved material is taken to a rapid moisture detector for detection to determine the moisture content thereof;
    第2步,取100g样品至聚四氟乙烯烧杯中,根据步骤1测得的样品含水率计算出样品中固相、液相含量,然后以固体重量单位为kg、液体体积单位为L,按照固液比1:20比例计算出权利要求1所述浸提液的体积,量取浸提液并将浸提液加入到烧杯中,人工快速搅拌5min;In the second step, 100g sample is taken into the polytetrafluoroethylene beaker, and the solid phase and liquid phase content in the sample are calculated according to the moisture content of the sample measured in step 1, and then the solid weight unit is kg, and the liquid volume unit is L, according to Calculating the volume of the extract according to claim 1 by the ratio of solid to liquid ratio of 1:20, measuring the extract and adding the extract to the beaker, and manually stirring for 5 min;
    第3步,将步骤2的烧杯置于恒温磁力搅拌器上,设置温度为40~70℃,转速为50~130r/min,搅拌时间为1~2h;In the third step, the beaker of step 2 is placed on a constant temperature magnetic stirrer, the set temperature is 40-70 ° C, the rotational speed is 50-130 r / min, and the stirring time is 1 ~ 2 h;
    第4步,通过0.45μm膜过滤后获得浸提液。 In the fourth step, the extract was obtained by filtration through a 0.45 μm membrane.
PCT/CN2017/073538 2017-02-14 2017-02-14 Leaching solution for waste incineration fly ash chelate and preparation and application methods therefor WO2018148869A1 (en)

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