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CN104692837A - Method of comprehensively utilizing sludge - Google Patents

Method of comprehensively utilizing sludge Download PDF

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Publication number
CN104692837A
CN104692837A CN201510079221.7A CN201510079221A CN104692837A CN 104692837 A CN104692837 A CN 104692837A CN 201510079221 A CN201510079221 A CN 201510079221A CN 104692837 A CN104692837 A CN 104692837A
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sludge
filter cake
activated carbon
comprehensive utilization
activator
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陈盛明
傅敏
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Chongqing Technology and Business University
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Chongqing Technology and Business University
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B17/00Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/342Preparation characterised by non-gaseous activating agents
    • C01B32/348Metallic compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

本发明公开了一种综合利用污泥的方法,包括以下步骤:1)氨氮回收:往脱水污泥中加入水,加热反应,将反应产生的气体溶解在水中,得到氨氮溶液,过滤反应物料,滤饼备用;2)制备鸟粪石肥料:往氨氮溶液中加入氯化镁溶液,再加入磷酸氢二钠溶液直至无沉淀产生,过滤,滤饼干燥后得到鸟粪石肥料;3)制备活性炭:将步骤1)得到的滤饼与活化剂和增碳剂混合、浸泡,然后加热烘干,干燥物质放入煅烧炉中煅烧,得到活性炭粗品;活性炭粗品用盐酸洗涤、过滤后,滤饼用水洗至中性,再烘干得到活性炭产品。本发明提取污泥中的氮、碳及金属元素,分别用于制备鸟粪石、活性炭和回收金属,实现了污泥的资源化综合利用,减少了环境污染。

The invention discloses a method for comprehensive utilization of sludge, which comprises the following steps: 1) recovery of ammonia nitrogen: adding water to dewatered sludge, heating and reacting, dissolving the gas generated by the reaction in water to obtain ammonia nitrogen solution, filtering the reaction materials, The filter cake is standby; 2) prepare struvite fertilizer: add magnesium chloride solution to the ammonia nitrogen solution, then add disodium hydrogen phosphate solution until no precipitation occurs, filter, and obtain struvite fertilizer after the filter cake is dried; 3) prepare activated carbon: Step 1) The obtained filter cake is mixed with an activator and a recarburizer, soaked, then heated and dried, and the dried material is put into a calciner for calcining to obtain a crude activated carbon product; the crude activated carbon product is washed with hydrochloric acid and filtered, and the filter cake is washed with water until neutral, and then dried to obtain activated carbon products. The invention extracts nitrogen, carbon and metal elements in the sludge, and uses them to prepare struvite, activated carbon and recover metals respectively, realizes comprehensive resource utilization of sludge, and reduces environmental pollution.

Description

一种综合利用污泥的方法A method for comprehensive utilization of sludge

技术领域technical field

本发明涉及污泥处理技术领域,具体涉及一种综合利用污泥的方法。The invention relates to the technical field of sludge treatment, in particular to a method for comprehensively utilizing sludge.

背景技术Background technique

污泥处理应以减量化、稳定化、无害化为处理目的。一般而言,污泥处理可供选择的方法大致有浓缩、消化脱水、焚烧、堆肥等,然后是最终处置。传统的污泥处置方式有填埋、焚烧、排海等。Sludge treatment should aim at reduction, stabilization and harmlessness. Generally speaking, the options for sludge treatment include concentration, digestion and dehydration, incineration, composting, etc., and then final disposal. Traditional sludge disposal methods include landfill, incineration, and sea discharge.

污泥中除了含有丰富的可以利用的氮、磷、钾多种微量元素和有机质,同时也含大量的病原体寄生虫(卵)、重金属和多种有毒有害有机污染物,如果不能妥善安全的处置,将给生态环境带来巨大的压力。In addition to rich nitrogen, phosphorus, potassium trace elements and organic matter that can be used in sludge, it also contains a large number of pathogen parasites (eggs), heavy metals and a variety of toxic and harmful organic pollutants. If it cannot be properly and safely disposed of , will bring enormous pressure to the ecological environment.

污泥处置最为经济有效的方式就是生物资源循环利用,即污泥资源利用处置,污泥的资源化利用主要是在农业、材料、能源方面的应用,这些方法在技术上是可行的,但是大多由于成本较高,工艺还不是很成熟,因此在实际处置过程中应用于工业处理还是较少。The most economical and effective way of sludge disposal is the recycling of biological resources, that is, the utilization and disposal of sludge resources. The resource utilization of sludge is mainly applied in agriculture, materials, and energy. These methods are technically feasible, but most of them are Due to the high cost and the immature technology, it is still rarely used in industrial treatment in the actual disposal process.

发明内容Contents of the invention

有鉴于此,本发明的目的在于提供一种综合利用污泥的方法,能够从污泥中制备鸟粪石肥料和活性炭,实现污泥的资源化利用,减少环境污染。In view of this, the purpose of the present invention is to provide a method for comprehensive utilization of sludge, which can prepare struvite fertilizer and activated carbon from sludge, realize resource utilization of sludge, and reduce environmental pollution.

为达到上述目的,本发明提供如下技术方案:To achieve the above object, the present invention provides the following technical solutions:

本发明的综合利用污泥的方法,包括以下步骤:The method for comprehensive utilization of sludge of the present invention comprises the following steps:

1)氨氮回收:往脱水污泥中加入水,用NaOH溶液调节体系pH值,加热反应,将反应产生的气体溶解在水中,得到氨氮溶液,过滤反应物料,滤饼备用;1) Ammonia nitrogen recovery: add water to the dewatered sludge, adjust the pH value of the system with NaOH solution, heat the reaction, dissolve the gas generated by the reaction in water to obtain ammonia nitrogen solution, filter the reaction material, and filter the cake for later use;

2)制备鸟粪石肥料:往步骤1)得到的氨氮溶液中加入氯化镁溶液,用NaOH溶液调节pH值,再加入磷酸氢二钠溶液直至无沉淀产生,过滤,滤饼干燥后得到鸟粪石肥料;2) Prepare struvite fertilizer: add magnesium chloride solution to the ammonia nitrogen solution obtained in step 1), adjust the pH value with NaOH solution, then add disodium hydrogen phosphate solution until no precipitation occurs, filter, and dry the filter cake to obtain struvite fertilizer;

3)制备活性炭:将步骤1)得到的滤饼与活化剂和增碳剂混合、浸泡,然后加热烘干,干燥物质放入煅烧炉中煅烧,得到活性炭粗品;活性炭粗品用盐酸洗涤、过滤后,滤饼用水洗至中性,再烘干得到活性炭产品。3) Prepare activated carbon: mix and soak the filter cake obtained in step 1) with an activator and a recarburizer, then heat and dry, put the dried material into a calciner and calcinate to obtain a crude activated carbon; the crude activated carbon is washed with hydrochloric acid and filtered , the filter cake is washed with water until neutral, and then dried to obtain activated carbon products.

进一步,所述步骤1)中,反应体系的pH值为9~13,反应温度为85~100℃,反应时间为2~4小时。Further, in the step 1), the pH value of the reaction system is 9-13, the reaction temperature is 85-100°C, and the reaction time is 2-4 hours.

进一步,所述步骤2)中,反应体系的pH值为7~11。Further, in the step 2), the pH value of the reaction system is 7-11.

进一步,所述步骤3)中,活化剂为氯化锌、硫酸、磷酸或氢氧化钠,增碳剂为玉米芯、秸秆、胶粉或煤矸石。Further, in the step 3), the activator is zinc chloride, sulfuric acid, phosphoric acid or sodium hydroxide, and the carburant is corn cob, straw, rubber powder or coal gangue.

进一步,所述步骤3)中,以重量计,增碳剂的用量为污泥用量的0.1~1倍,活化剂的用量为污泥用量的1.5~6倍,活化剂的质量浓度为20%~70%,煅烧温度为200~500℃,煅烧时间为30~70分钟。Further, in the step 3), by weight, the amount of the carburant is 0.1 to 1 times the amount of the sludge, the amount of the activator is 1.5 to 6 times the amount of the sludge, and the mass concentration of the activator is 20% ~70%, the calcination temperature is 200-500°C, and the calcination time is 30-70 minutes.

进一步,所述步骤1)和步骤2)中,滤液均循环用于配制NaOH溶液。Further, in the step 1) and step 2), the filtrate is circulated for preparing NaOH solution.

进一步,所述步骤3)中,煅烧产生的尾气用于烘干滤饼与活化剂和增碳剂的混合液。Further, in the step 3), the tail gas generated by calcination is used to dry the mixed liquid of filter cake, activator and recarburizer.

进一步,所述步骤3)中,盐酸洗涤活性炭粗品后产生的含酸废水用NaOH溶液中和至中性,过滤,滤饼经干燥后得到碱式金属混合物。Further, in the step 3), the acid-containing wastewater produced after washing the crude activated carbon with hydrochloric acid is neutralized to neutral with NaOH solution, filtered, and the filter cake is dried to obtain a mixture of basic metals.

本发明的有益效果在于:The beneficial effects of the present invention are:

本发明是将污泥作为资源利用的方法,提取污泥中的氮、碳及金属元素,分别用于制备鸟粪石、活性炭和回收金属,实现了污泥的资源化综合利用,减少了环境污染;并且本发明中,废水能够得到循环回用,尾气中的热能可以回收利用,节能减排效益明显。The invention is a method of using sludge as a resource, extracting nitrogen, carbon and metal elements in the sludge, and using them to prepare struvite, activated carbon and recovering metals respectively, realizing the comprehensive utilization of sludge resources and reducing environmental pollution. pollution; and in the present invention, the waste water can be recycled, the heat energy in the tail gas can be recycled, and the benefits of energy saving and emission reduction are obvious.

附图说明Description of drawings

为了使本发明的目的、技术方案和有益效果更加清楚,本发明提供如下附图进行说明:In order to make the purpose, technical scheme and beneficial effect of the present invention clearer, the present invention provides the following drawings for illustration:

图1为本发明的综合利用污泥的方法的工艺流程图。Fig. 1 is the process flow diagram of the method for comprehensive utilization of sludge of the present invention.

具体实施方式Detailed ways

下面将结合附图,对本发明的优选实施例进行详细的描述。The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

图1为本发明的综合利用污泥的方法的工艺流程图,如图所示,本发明的综合利用污泥的方法包括以下步骤:Fig. 1 is the process flow chart of the method for comprehensively utilizing sludge of the present invention, as shown in the figure, the method for comprehensively utilizing sludge of the present invention comprises the following steps:

1)氨氮回收:往脱水污泥中加入水,用NaOH溶液调节体系pH值,加热反应,将反应产生的气体溶解在水中,得到氨氮溶液,过滤反应物料,滤饼备用,滤液循环用于配制NaOH溶液;1) Ammonia nitrogen recovery: add water to the dewatered sludge, adjust the pH value of the system with NaOH solution, heat the reaction, dissolve the gas generated by the reaction in water to obtain ammonia nitrogen solution, filter the reaction material, filter cake for standby, and circulate the filtrate for preparation NaOH solution;

2)制备鸟粪石肥料:往步骤1)得到的氨氮溶液中加入氯化镁溶液,用NaOH溶液调节pH值,再加入磷酸氢二钠溶液直至无沉淀产生,过滤,滤饼干燥后得到鸟粪石肥料,滤液循环用于配制NaOH溶液;2) Prepare struvite fertilizer: add magnesium chloride solution to the ammonia nitrogen solution obtained in step 1), adjust the pH value with NaOH solution, then add disodium hydrogen phosphate solution until no precipitation occurs, filter, and dry the filter cake to obtain struvite Fertilizer, filtrate circulation is used to prepare NaOH solution;

3)制备活性炭:将步骤1)得到的滤饼与活化剂和增碳剂混合、浸泡,然后加热烘干,干燥物质放入煅烧炉中煅烧,得到活性炭粗品,煅烧产生的尾气用于烘干滤饼与活化剂和增碳剂的混合液;活性炭粗品用盐酸洗涤、过滤后,滤饼用水洗至中性,再烘干得到活性炭产品;盐酸洗涤活性炭粗品后产生的含酸废水用NaOH溶液中和至中性,过滤,滤饼经干燥后得到碱式金属混合物。3) Preparation of activated carbon: mix and soak the filter cake obtained in step 1) with an activator and a recarburizer, then heat and dry, put the dried material into a calciner for calcination to obtain a crude activated carbon, and use the tail gas generated by calcination for drying The mixture of filter cake, activator and recarburizer; the crude activated carbon is washed with hydrochloric acid and filtered, the filter cake is washed with water until neutral, and then dried to obtain activated carbon products; the acid-containing wastewater produced after washing the crude activated carbon with hydrochloric acid is treated with NaOH solution Neutralize to neutral, filter, and dry the filter cake to obtain a basic metal mixture.

本发明各个具体实施例的工艺参数及结果如下:Process parameter and result of each specific embodiment of the present invention are as follows:

1、污泥提取氨氮1. Extraction of ammonia nitrogen from sludge

不同条件下,污泥中提取氨氮量Under different conditions, the amount of ammonia nitrogen extracted from sludge

注:在氨气出口处用30mL蒸馏水吸收氨气。Note: Absorb ammonia gas with 30mL distilled water at the outlet of ammonia gas.

2、制备鸟粪石肥料2. Preparation of struvite fertilizer

利用污泥中提取氨氮制备鸟粪石肥料Preparation of struvite fertilizer by extracting ammonia nitrogen from sludge

3、制备活性炭3. Preparation of activated carbon

3.1不同活化剂对污泥制备活性炭的影响3.1 Effects of different activators on the preparation of activated carbon from sludge

不同活化剂,污泥制备活性炭情况Different activators, sludge preparation of activated carbon

3.2不同增碳剂对污泥制备活性炭的影响3.2 Effects of different recarburizers on the preparation of activated carbon from sludge

不同增碳剂,污泥制备活性炭情况Preparation of activated carbon from different carburizers and sludge

3.3增碳剂用量对污泥制备活性炭的影响3.3 The effect of the amount of carburant on the preparation of activated carbon from sludge

不同增碳剂用量下,污泥制备活性炭情况Preparation of activated carbon from sludge under different carburant dosage

3.4煅烧温度对污泥制备活性炭的影响3.4 Effect of calcination temperature on the preparation of activated carbon from sludge

不同煅烧温度下,污泥制备活性炭情况Preparation of activated carbon from sludge at different calcination temperatures

3.5活化剂浓度对污泥制备活性炭的影响3.5 Effect of activator concentration on the preparation of activated carbon from sludge

不同活化剂浓度下,污泥制备活性炭情况Preparation of activated carbon from sludge under different activator concentrations

3.6煅烧时间对污泥制备活性炭的影响3.6 The effect of calcination time on the preparation of activated carbon from sludge

不同煅烧时间下,污泥制备活性炭情况Preparation of activated carbon from sludge at different calcination times

3.7活化剂用量对污泥制备活性炭的影响3.7 The effect of the amount of activator on the preparation of activated carbon from sludge

不同活化剂用量下,污泥制备活性炭情况Preparation of activated carbon from sludge under different activator dosage

最后说明的是,以上优选实施例仅用以说明本发明的技术方案而非限制,尽管通过上述优选实施例已经对本发明进行了详细的描述,但本领域技术人员应当理解,可以在形式上和细节上对其作出各种各样的改变,而不偏离本发明权利要求书所限定的范围。Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail through the above preferred embodiments, those skilled in the art should understand that it can be described in terms of form and Various changes may be made in the details without departing from the scope of the invention defined by the claims.

Claims (8)

1. fully utilize a method for mud, it is characterized in that: comprise the following steps:
1) ammonia nitrogen reclaims: in dewatered sludge, add water, and by NaOH solution regulation system pH value, reacting by heating, gas dissolving reaction produced, in water, obtains ammonia nitrogen solution, and filter reaction mass, filter cake is for subsequent use;
2) struvite fertilizer is prepared: toward step 1) add magnesium chloride solution in the ammonia nitrogen solution that obtains, use NaOH solution adjust ph, then add disodium phosphate soln until produce without precipitation, filter, after filtration cakes torrefaction, obtain struvite fertilizer;
3) gac is prepared: by step 1) filter cake that obtains mixes with activator and carburelant, soaks, then heating, drying, and dry substance is put into calcining furnace and is calcined, and obtains gac crude product; After gac crude product salt acid elution, filtration, filter cake washes with water to neutrality, then oven dry obtains activated carbon product.
2. the method for comprehensive utilization mud according to claim 1, is characterized in that: described step 1) in, the pH value of reaction system is 9 ~ 13, and temperature of reaction is 85 ~ 100 DEG C, and the reaction times is 2 ~ 4 hours.
3. the method for comprehensive utilization mud according to claim 1, is characterized in that: described step 2) in, the pH value of reaction system is 7 ~ 11.
4. the method for comprehensive utilization mud according to claim 1, is characterized in that: described step 3) in, activator is zinc chloride, sulfuric acid, phosphoric acid or sodium hydroxide, and carburelant is corn cob, stalk, rubber powder or coal gangue.
5. the method for comprehensive utilization mud according to claim 1, it is characterized in that: described step 3) in, by weight, the consumption of carburelant is 0.1 ~ 1 times of mud consumption, the consumption of activator is 1.5 ~ 6 times of mud consumption, the mass concentration of activator is 20% ~ 70%, and calcining temperature is 200 ~ 500 DEG C, and calcination time is 30 ~ 70 minutes.
6. the method for comprehensive utilization mud according to claim 1, is characterized in that: described step 1) and step 2) in, filtrate is all cycled to used in preparation NaOH solution.
7. the method for comprehensive utilization mud according to claim 1, is characterized in that: described step 3) in, the tail gas that calcining produces is for drying the mixed solution of filter cake and activator and carburelant.
8. the method for comprehensive utilization mud according to claim 1, it is characterized in that: described step 3) in, the acid-bearing wastewater NaOH solution produced after hydrochloric acid detergent active charcoal crude product is neutralized to neutrality, and filter, filter cake obtains basic metal mixture after drying.
CN201510079221.7A 2015-02-13 2015-02-13 Method of comprehensively utilizing sludge Pending CN104692837A (en)

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CN114058848A (en) * 2021-10-09 2022-02-18 杭州逐真科技有限公司 System and process for recovering copper, nickel, zinc, chromium and iron from electroplating sludge or other multi-metal mixture

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CN106025296A (en) * 2016-07-27 2016-10-12 同济大学 Nitrogen-phosphorus double-doped carbon material as well as preparation method and application thereof
CN113277690A (en) * 2021-05-12 2021-08-20 华中科技大学 Method and product for comprehensive treatment of sludge and recovery of phosphorus resources
CN114058848A (en) * 2021-10-09 2022-02-18 杭州逐真科技有限公司 System and process for recovering copper, nickel, zinc, chromium and iron from electroplating sludge or other multi-metal mixture

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