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CN116639657A - A kind of hydrochloric acid purifying treatment method containing sulfuric acid impurity - Google Patents

A kind of hydrochloric acid purifying treatment method containing sulfuric acid impurity Download PDF

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Publication number
CN116639657A
CN116639657A CN202310772220.5A CN202310772220A CN116639657A CN 116639657 A CN116639657 A CN 116639657A CN 202310772220 A CN202310772220 A CN 202310772220A CN 116639657 A CN116639657 A CN 116639657A
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hydrochloric acid
sulfuric acid
evaporator
absorption tower
containing sulfuric
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徐书建
韩景城
韩永胜
何亚磊
王美
徐彦峰
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Henan Hdf Chemical Co ltd
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Henan Hdf Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/01Chlorine; Hydrogen chloride
    • C01B7/07Purification ; Separation
    • C01B7/0706Purification ; Separation of hydrogen chloride
    • C01B7/0712Purification ; Separation of hydrogen chloride by distillation
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

本发明公开了一种含硫酸杂质的盐酸净化处理方法,在一定温度条件下,对含硫酸杂质的盐酸进行蒸馏,蒸出的氯化氢气体和水蒸气经冷凝后并吸收产生新盐酸,其中蒸发后的硫酸浓缩液留在蒸发器中,收集之后进一步处理利用,通过此过程达到净化处理含硫酸杂质的盐酸的目的;本发明具有有效除去硫酸、净化盐酸、提高盐酸利用率、连续性强、安全环保的优点。

The invention discloses a method for purifying hydrochloric acid containing sulfuric acid impurities. Under certain temperature conditions, the hydrochloric acid containing sulfuric acid impurities is distilled, and the distilled hydrogen chloride gas and water vapor are condensed and absorbed to produce new hydrochloric acid. The concentrated solution of sulfuric acid remains in the evaporator, and is further processed and utilized after being collected. Through this process, the purpose of purifying hydrochloric acid containing sulfuric acid impurities is achieved; the present invention has the functions of effectively removing sulfuric acid, purifying hydrochloric acid, improving the utilization rate of hydrochloric acid, strong continuity, and safety. The advantages of environmental protection.

Description

一种含硫酸杂质的盐酸净化处理方法A kind of hydrochloric acid purifying treatment method containing sulfuric acid impurity

技术领域technical field

本发明涉及一种盐酸净化处理的方法,具体涉及一种含硫酸杂质的盐酸净化处理方法。The invention relates to a method for purifying hydrochloric acid, in particular to a method for purifying hydrochloric acid containing sulfuric acid impurities.

背景技术Background technique

盐酸是氯化氢(HCL)的水溶液,属于一元无机强酸,盐酸的性状为无色透明液体,有强烈刺鼻气味,具有较高腐蚀性,具有极强的挥发性,多作为工业原料来使用,应用越来越广泛。但在实际生产中,一些副产盐酸由于含有较多杂质很难被利用,如在硫磺催化法合成一氯乙酸的过程中,产生的副产盐酸中含有较多的硫酸盐,含量高达1%以上,作为工业原料有较大的弊端,影响产品品质,很难应用到生产中去,导致含硫酸的盐酸利用率越来越低,造成了严重的资源浪费和处理压力,对生产和环境都有一定的影响,因此需要对含硫酸的盐酸需要进行净化处理,来达到资源循环使用的目的。Hydrochloric acid is an aqueous solution of hydrogen chloride (HCL), which is a monobasic inorganic strong acid. The properties of hydrochloric acid are colorless and transparent liquid, with a strong pungent smell, high corrosiveness, and strong volatility. It is mostly used as industrial raw materials. Applications more and more widely. However, in actual production, some by-product hydrochloric acid is difficult to be utilized because it contains more impurities. For example, in the process of synthesizing monochloroacetic acid by sulfur catalysis, the by-product hydrochloric acid contains more sulfate, with a content as high as 1%. As mentioned above, as an industrial raw material, it has great disadvantages, affects product quality, and is difficult to apply to production, resulting in lower and lower utilization of hydrochloric acid containing sulfuric acid, resulting in serious waste of resources and processing pressure, which is harmful to both production and the environment. There is a certain impact, so it is necessary to purify the hydrochloric acid containing sulfuric acid to achieve the purpose of resource recycling.

现有的净化处理含硫酸的盐酸方法和装置很多,大多数采用的方法是沉淀法,即添加化学试剂与硫酸根反应并形成沉淀,此类化学试剂主要为氯化钡、氯化钙等,其中,氯化钡成本太高,不适合工业化处理,因此在工业上主要采用的氯化钙沉淀法,利用钙离子与硫酸根反应生产微溶的硫酸钙沉淀,再进一步过滤除杂即可,但是在利用氯化钙处理过程中,由于氯化钙是微溶物质,导致盐酸中的硫酸根处理的不够彻底,净化处理后的盐酸硫酸根含量仍在在0.1%左右,造成盐酸中硫酸杂质含量仍较高,在一些对盐酸品质控制要求较高的领域,依旧无法使用,需要对含硫酸杂质盐酸继续净化处理,才能实现资源循环使用,因此需要继续改进盐酸净化处理技术,特别是含硫酸杂质含量高的盐酸净化处理方法,降低硫酸含量,实现盐酸的循环使用。There are many existing methods and devices for purifying hydrochloric acid containing sulfuric acid, most of which are precipitation methods, that is, adding chemical reagents to react with sulfate radicals and form precipitates. Such chemical reagents are mainly barium chloride, calcium chloride, etc. Among them, the cost of barium chloride is too high to be suitable for industrialized treatment. Therefore, the calcium chloride precipitation method mainly used in industry uses calcium ions to react with sulfate radicals to produce slightly soluble calcium sulfate precipitates, and then further filter to remove impurities. However, in the process of using calcium chloride to treat, since calcium chloride is a slightly soluble substance, the treatment of sulfate radicals in hydrochloric acid is not thorough enough, and the sulfate radical content of hydrochloric acid after purification treatment is still around 0.1%, resulting in sulfuric acid impurities in hydrochloric acid The content of hydrochloric acid is still relatively high, and it is still unusable in some fields that require high quality control of hydrochloric acid. It is necessary to continue to purify hydrochloric acid containing sulfuric acid impurities in order to realize resource recycling. Therefore, it is necessary to continue to improve hydrochloric acid purification technology, especially hydrochloric acid containing sulfuric acid. The hydrochloric acid purification treatment method with high impurity content reduces the content of sulfuric acid and realizes the recycling of hydrochloric acid.

所以,为解决上述问题,开发一种含硫酸杂质的盐酸净化处理方法很有必要。Therefore, in order to solve the above problems, it is necessary to develop a method for purifying hydrochloric acid containing sulfuric acid impurities.

发明内容Contents of the invention

本发明的目的是为了克服现有技术的不足,而提供一种含硫酸杂质的盐酸净化处理方法,降低盐酸中的硫酸杂质,实现含硫酸杂质的盐酸再利用。The purpose of the present invention is in order to overcome the deficiencies in the prior art, and provide a kind of hydrochloric acid purification treatment method containing sulfuric acid impurities, reduce the sulfuric acid impurities in hydrochloric acid, realize the hydrochloric acid containing sulfuric acid impurities reuse.

本发明的目的是这样实现的:一种含硫酸杂质的盐酸净化处理方法,包括以下步骤:The object of the present invention is achieved in that a kind of hydrochloric acid purifying treatment method containing sulfuric acid impurity comprises the following steps:

S01、将含硫酸杂质的盐酸物料进入到蒸发器进行加热蒸发,控制蒸发器内物料温度在90-105℃,保持蒸发器内液位在蒸发器的三分之二容积左右;S01. Enter the hydrochloric acid material containing sulfuric acid impurities into the evaporator for heating and evaporation, control the temperature of the material in the evaporator at 90-105°C, and keep the liquid level in the evaporator at about two-thirds of the volume of the evaporator;

S02、经蒸发器蒸发后的水蒸气和氯化氢气体进入到冷凝器中,经蒸发器蒸发后的浓缩液在硫酸含量达到30%以上后,进行放料,然后将其进一步浓缩为含量为98%以上的浓硫酸,用作其他工业原料;S02. The water vapor and hydrogen chloride gas evaporated by the evaporator enter the condenser, and the concentrated liquid evaporated by the evaporator is discharged after the sulfuric acid content reaches more than 30%, and then it is further concentrated to a content of 98%. The above concentrated sulfuric acid is used as other industrial raw materials;

S03、进入到冷凝器中的水蒸气和氯化氢气体在冷凝器中进行冷却,其中经冷凝器冷却后的水蒸气产生的水吸收部分氯化氢气体形成稀盐酸;S03, the water vapor and hydrogen chloride gas entering the condenser are cooled in the condenser, wherein the water produced by the water vapor cooled by the condenser absorbs part of the hydrogen chloride gas to form dilute hydrochloric acid;

S04、冷却后的氯化氢气体和形成的稀盐酸进入到盐酸吸收塔中吸收,吸收后的盐酸含量合格后连续采出,其中,步骤S01中的进料盐酸与采出的盐酸的质量比例控制在1:0.94-0.96。S04, the hydrogen chloride gas after cooling and the dilute hydrochloric acid that forms enter in the hydrochloric acid absorption tower and absorb, and the hydrochloric acid content after the absorption is qualified and continuously extracted, and wherein, the mass ratio of the hydrochloric acid of feed in the step S01 and the hydrochloric acid of extraction is controlled at 1:0.94-0.96.

进一步地,所述蒸发器采用蒸汽加热,所述蒸发器连接有进料泵、液体流量计和控制阀门。Further, the evaporator is heated by steam, and the evaporator is connected with a feed pump, a liquid flow meter and a control valve.

进一步地,所述蒸发器上还设置有在线测定装置和视镜。Further, the evaporator is also provided with an online measurement device and a sight glass.

进一步地,所述冷凝器的进料管道上还设置有气体流量计和控制阀门。Further, a gas flow meter and a control valve are also provided on the feed pipeline of the condenser.

进一步地,所述盐酸吸收塔采用两级吸收,包括一级吸收塔和二级吸收塔,所述一级吸收塔顶端的气相出口连接二级吸收塔,二级吸收塔的气相出口连接有氯化氢气体测定装置,二级吸收塔吸收后的盐酸合格后连续采出。Further, the hydrochloric acid absorption tower adopts two-stage absorption, including a primary absorption tower and a secondary absorption tower, the gas phase outlet at the top of the primary absorption tower is connected to the secondary absorption tower, and the gas phase outlet of the secondary absorption tower is connected with hydrogen chloride Gas measuring device, after the hydrochloric acid absorbed by the secondary absorption tower is qualified, it is continuously extracted.

进一步地,所述盐酸吸收塔上设置有强制循环泵将塔釜内的稀盐酸在塔体和塔釜之间循环。Further, the hydrochloric acid absorption tower is provided with a forced circulation pump to circulate the dilute hydrochloric acid in the tower bottom between the tower body and the tower bottom.

进一步地,所述盐酸吸收塔上设置有酸度测定装置。Further, the hydrochloric acid absorption tower is provided with an acidity measuring device.

由于采用了上述技术方案,本发明的有益效果是:Owing to adopted above-mentioned technical scheme, the beneficial effect of the present invention is:

(1)通过在常压和一定温度条件下,对含硫酸杂质的盐酸进行蒸发再吸收,达到净化处理含硫酸杂质的盐酸的目的,可将盐酸中硫酸含量降至0.001%以下,且盐酸含量降低不足0.5%,有效除去硫酸,净化盐酸,满足其他很多工业原料的需求,有效提高盐酸利用率,同时可进行连续进料和连续采出,实行连续处理,处理过程简单,危险系数小,处理效果明显;(1) By evaporating and reabsorbing hydrochloric acid containing sulfuric acid impurities under normal pressure and certain temperature conditions, the purpose of purifying and treating hydrochloric acid containing sulfuric acid impurities can be achieved, and the content of sulfuric acid in hydrochloric acid can be reduced to below 0.001%, and the content of hydrochloric acid The reduction is less than 0.5%, effectively removes sulfuric acid, purifies hydrochloric acid, meets the needs of many other industrial raw materials, effectively improves the utilization rate of hydrochloric acid, and can carry out continuous feeding and continuous extraction at the same time, and implements continuous treatment. The treatment process is simple, the risk factor is small, and the treatment The effect is obvious;

(2)通过将盐酸吸收塔分为两级吸收,且使用强制循环泵将塔釜内稀盐酸在塔体和塔釜之间循环,吸收更彻底,减少资源浪费,同时处理过程中无残留,处理彻底,安全环保。(2) By dividing the hydrochloric acid absorption tower into two stages of absorption, and using a forced circulation pump to circulate dilute hydrochloric acid in the tower kettle between the tower body and the tower kettle, the absorption is more thorough, the waste of resources is reduced, and there is no residue during the treatment process. Thorough treatment, safe and environmentally friendly.

附图说明Description of drawings

图1是本发明的流程框图。Fig. 1 is a flowchart of the present invention.

实施方式Implementation

下面通过实施例,并结合附图,对本发明的技术方案做进一步具体的说明。The technical solutions of the present invention will be further specifically described below through embodiments and in conjunction with the accompanying drawings.

如图1所示,一种含硫酸杂质的盐酸净化处理方法,具体包括以下步骤:As shown in Figure 1, a kind of hydrochloric acid purifying treatment method containing sulfuric acid impurity specifically comprises the following steps:

S01、将含硫酸杂质的盐酸物料进入到蒸发器进行加热蒸发,控制蒸发器内物料温度在90-105℃,保持蒸发器内液位在蒸发器的三分之二容积左右;S01. Enter the hydrochloric acid material containing sulfuric acid impurities into the evaporator for heating and evaporation, control the temperature of the material in the evaporator at 90-105°C, and keep the liquid level in the evaporator at about two-thirds of the volume of the evaporator;

S02、经蒸发器蒸发后的水蒸气和氯化氢气体进入到冷凝器中,经蒸发器蒸发后的浓缩液在硫酸含量达到30%以上后,进行放料,然后将其进一步浓缩为含量为98%以上的浓硫酸,用作其他工业原料;S02. The water vapor and hydrogen chloride gas evaporated by the evaporator enter the condenser, and the concentrated liquid evaporated by the evaporator is discharged after the sulfuric acid content reaches more than 30%, and then it is further concentrated to a content of 98%. The above concentrated sulfuric acid is used as other industrial raw materials;

S03、进入到冷凝器中的水蒸气和氯化氢气体在冷凝器中进行冷却,其中经冷凝器冷却后的水蒸气产生的水吸收部分氯化氢气体形成稀盐酸;S03, the water vapor and hydrogen chloride gas entering the condenser are cooled in the condenser, wherein the water produced by the water vapor cooled by the condenser absorbs part of the hydrogen chloride gas to form dilute hydrochloric acid;

S04、冷却后的氯化氢气体和形成的稀盐酸进入到盐酸吸收塔中吸收,吸收后的盐酸含量合格后连续采出,其中,步骤S01中的进料盐酸与采出的盐酸的质量比例控制在1:0.94-0.96。S04, the hydrogen chloride gas after cooling and the dilute hydrochloric acid that forms enter in the hydrochloric acid absorption tower and absorb, and the hydrochloric acid content after the absorption is qualified and continuously extracted, and wherein, the mass ratio of the hydrochloric acid of feed in the step S01 and the hydrochloric acid of extraction is controlled at 1:0.94-0.96.

具体的,所述蒸发器的蒸发室可以采用蒸汽加热,蒸发温度控制在90-105℃,沸腾明显,蒸发较快,同时,为了避免热量的散失和提高加热效率,所述蒸发器上还设置有夹层和保温装置;含硫酸杂质的盐酸物料通过进料泵进入到蒸发器中,同时设置有液体流量计和控制阀门,便于控制进料速率,通过控制进料速率,可保持物料的液位在蒸发器的三分之二容积处;所述蒸发器上设置有视镜,用于对蒸发器内物料液位进行观测;同时所述蒸发器上还设置有在线测定装置,用于对蒸发器内部浓缩液硫酸浓度进行测定;优选的,为了加快蒸发效率,盐酸物料在进料时还可以通过液体分布器进入到蒸发器内。Specifically, the evaporation chamber of the evaporator can be heated by steam, the evaporation temperature is controlled at 90-105°C, the boiling is obvious, and the evaporation is fast. At the same time, in order to avoid heat loss and improve heating efficiency, the evaporator is also equipped with There are interlayers and insulation devices; the hydrochloric acid material containing sulfuric acid impurities enters the evaporator through the feed pump, and a liquid flow meter and control valve are installed at the same time to facilitate the control of the feed rate. By controlling the feed rate, the liquid level of the material can be maintained. At two-thirds of the volume of the evaporator; the evaporator is provided with a sight glass for observing the liquid level of the material in the evaporator; The sulfuric acid concentration of the concentrate inside the evaporator is measured; preferably, in order to speed up the evaporation efficiency, the hydrochloric acid material can also enter the evaporator through the liquid distributor when feeding.

具体的,所述冷凝器的进料管道上还设置有气体流量计和控制阀门,便于控制冷凝器的进料速率。Specifically, the feed pipeline of the condenser is also provided with a gas flow meter and a control valve to facilitate the control of the feed rate of the condenser.

具体的,经冷却后的氯化氢气体可以通过气体分布器进入到盐酸吸收塔内部,气体分布器可以设置于盐酸吸收塔内部稀盐酸的液面以下,吸收更充分;所述盐酸吸收塔上设置有强制循环泵将塔釜内的稀盐酸在塔体和塔釜之间循环,吸收更彻底,减少资源浪费,进一步地,由于氯化氢气体在吸收过程中会放热,因此,在循环时还可以设置有冷凝装置,对循环的吸收液进行冷却;所述盐酸吸收塔上还设置有酸度测定装置,对塔釜内的盐酸含量进行测定。Specifically, the hydrogen chloride gas after cooling can enter the inside of the hydrochloric acid absorption tower through the gas distributor, and the gas distributor can be arranged below the liquid level of dilute hydrochloric acid inside the hydrochloric acid absorption tower to absorb more fully; the hydrochloric acid absorption tower is provided with The forced circulation pump circulates the dilute hydrochloric acid in the tower kettle between the tower body and the tower kettle, so that the absorption is more thorough and the waste of resources is reduced. Furthermore, since the hydrogen chloride gas will release heat during the absorption process, it can also be set during circulation. There is a condensing device to cool the circulating absorption liquid; the hydrochloric acid absorption tower is also equipped with an acidity measuring device to measure the hydrochloric acid content in the tower kettle.

具体的,所述盐酸吸收塔采用两级吸收,包括一级吸收塔和二级吸收塔,所述一级吸收塔顶端的气相出口连接二级吸收塔,通过二级吸收塔对一级吸收塔排出的氯化氢气体进行进一步地吸收,二级吸收塔的气相出口连接有氯化氢气体测定装置,通过氯化氢气体测定装置对排出的气体进行测定,保证吸收的更加彻底,减少资源浪费,同时也避免了排出的气体中存在残留,更加安全环保,同时在二级吸收塔吸收后的盐酸合格后连续采出。Specifically, the hydrochloric acid absorption tower adopts two-stage absorption, including a primary absorption tower and a secondary absorption tower, the gas phase outlet at the top of the primary absorption tower is connected to the secondary absorption tower, and the primary absorption tower The discharged hydrogen chloride gas is further absorbed, and the gas phase outlet of the secondary absorption tower is connected with a hydrogen chloride gas measuring device, and the discharged gas is measured by the hydrogen chloride gas measuring device to ensure more thorough absorption, reduce waste of resources, and avoid discharge There are residues in the gas, which is safer and more environmentally friendly. At the same time, the hydrochloric acid absorbed by the secondary absorption tower is continuously extracted after passing the qualification.

应说明的是,在本申请中,所采用的蒸发器、冷凝器、盐酸吸收塔及管件等结构,应采用耐盐酸材料来实现,如所述盐酸吸收塔和进料泵以及相关管件等可以采用pp材质或者内衬四氟,所述蒸发器和冷凝器可以采用石墨材质,这均属于现有技术,对于本领域技术人员来说属于公知常识,故在此不再做具体限定。It should be noted that in this application, the structures of the evaporator, condenser, hydrochloric acid absorption tower and pipe fittings used should be realized by using hydrochloric acid resistant materials, such as the hydrochloric acid absorption tower, feed pump and related pipe fittings, etc. Using pp material or lined with tetrafluoroethylene, the evaporator and condenser can be made of graphite material, which belongs to the prior art and is common knowledge for those skilled in the art, so no specific limitation is made here.

本发明具体实施时,作为本发明的实施例一,在本实施例中,进料物料含硫酸杂质的盐酸中盐酸含量32.0%,硫酸含量为1.2%,小型实验净化处理装置准备完全后,开始进料,并开始加热蒸发器,蒸发器内液体温度稳定在90℃,液位控制在蒸发器容积的三分之二左右,稳定后,含硫酸杂质的盐酸进料量为1000g每小时,二级吸收塔内加入吸收水,一级吸收塔内盐酸含量达到31.0%以上开始采出处理后盐酸,每小时采出处理后盐酸940g,二级吸收塔氯化氢测定装置显示为0㎎/L,采出的处理后的盐酸中盐酸含量为31.8%,硫酸含量为0.0001%。When the present invention was implemented, as Embodiment 1 of the present invention, in this embodiment, the hydrochloric acid content in the hydrochloric acid containing sulfuric acid impurity in the feed material was 32.0%, and the sulfuric acid content was 1.2%. After the small-scale experimental purification treatment device was fully prepared, start Feed the material and start heating the evaporator. The temperature of the liquid in the evaporator is stabilized at 90°C, and the liquid level is controlled at about two-thirds of the volume of the evaporator. After stabilization, the feed rate of hydrochloric acid containing sulfuric acid impurities is 1000g per hour, two Absorption water is added into the first-stage absorption tower, and the hydrochloric acid content in the first-stage absorption tower reaches more than 31.0%, and the treated hydrochloric acid is extracted, and 940g of the treated hydrochloric acid is produced every hour, and the hydrogen chloride measuring device of the second-stage absorption tower shows 0㎎/L, and the output is 0㎎/L. The content of hydrochloric acid in the treated hydrochloric acid is 31.8%, and the content of sulfuric acid is 0.0001%.

作为本发明的实施例二,在本实施例中,进料物料含硫酸杂质的盐酸中盐酸含量33.5%,硫酸含量为1.3%,小型实验净化处理装置准备完全后,开始进料,并开始加热蒸发器,蒸发器内液体温度稳定在98℃,液位控制在蒸发器容积的三分之二左右,稳定后,含硫酸杂质的盐酸进料量为1000g每小时,二级吸收塔内加入吸收水,一级吸收塔内盐酸含量达到31.0%以上开始采出处理后盐酸,每小时采出处理后盐酸953g,二级吸收塔氯化氢测定装置显示为0㎎/L,采出的处理后的盐酸中盐酸含量为33.2.%,硫酸含量为0.0003%。As the second embodiment of the present invention, in this embodiment, the content of hydrochloric acid in the hydrochloric acid containing sulfuric acid impurities in the feed material is 33.5%, and the content of sulfuric acid is 1.3%. After the small-scale experimental purification treatment device is fully prepared, start feeding and start heating Evaporator, the temperature of the liquid in the evaporator is stabilized at 98°C, and the liquid level is controlled at about two-thirds of the volume of the evaporator. After stabilization, the feed rate of hydrochloric acid containing sulfuric acid impurities is 1000g per hour, and absorption is added to the secondary absorption tower Water, when the hydrochloric acid content in the primary absorption tower reaches 31.0% or more, the treated hydrochloric acid is extracted, and 953g of treated hydrochloric acid is produced per hour, and the hydrogen chloride measuring device in the secondary absorption tower shows 0㎎/L. The content of hydrochloric acid in medium is 33.2.%, and the content of sulfuric acid is 0.0003%.

作为本发明的实施例三,在本实施例中,进料物料含硫酸杂质的盐酸中盐酸含量35.0%,硫酸含量为1.5%,小型实验净化处理装置准备完全后,开始进料,并开始加热蒸发器,蒸发器内液体温度稳定在105℃,液位控制在蒸发器容积的三分之二左右,稳定后,含硫酸杂质的盐酸进料量为1000g每小时,二级吸收塔内加入吸收水,一级吸收塔内盐酸含量达到31.0%以上开始采出处理后盐酸,每小时采出处理后盐酸960g,二级吸收塔氯化氢测定装置显示为0㎎/L,采出的处理后的盐酸中盐酸含量为34.6%,硫酸含量为0.0002%。As embodiment three of the present invention, in this embodiment, the content of hydrochloric acid in the hydrochloric acid containing sulfuric acid impurities in the feed material is 35.0%, and the content of sulfuric acid is 1.5%. After the small-scale experimental purification treatment device is fully prepared, start feeding and start heating Evaporator, the temperature of the liquid in the evaporator is stabilized at 105°C, and the liquid level is controlled at about two-thirds of the volume of the evaporator. After stabilization, the feed rate of hydrochloric acid containing sulfuric acid impurities is 1000g per hour, and absorption is added to the secondary absorption tower Water, when the hydrochloric acid content in the first-stage absorption tower reaches more than 31.0%, the treated hydrochloric acid is extracted, and 960g of treated hydrochloric acid is produced per hour. The content of hydrochloric acid in medium is 34.6%, and the content of sulfuric acid is 0.0002%.

最后应说明的是,以上实施例仅用以说明本发明的技术方案,而非对其限制,尽管参照上述实施例对本发明进行了详细的说明,所属领域的普通技术人员应当理解,依然可以对本发明的具体实施方式进行修改或者等同替换,而未脱离本发明精神和范围的任何修改或者等同替换,其均应涵盖在本发明的权利要求范围当中。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than limit them. Although the present invention has been described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that the present invention can still be The specific implementation of the invention is modified or equivalently replaced, and any modification or equivalently replaced without departing from the spirit and scope of the present invention shall be covered by the claims of the present invention.

Claims (7)

1. A hydrochloric acid purification treatment method containing sulfuric acid impurities is characterized in that: the method comprises the following steps:
s01, feeding hydrochloric acid materials containing sulfuric acid impurities into an evaporator for heating and evaporating, controlling the temperature of the materials in the evaporator to be 90-105 ℃, and keeping the liquid level in the evaporator to be about two thirds of the volume of the evaporator;
s02, enabling the water vapor and the hydrogen chloride gas evaporated by the evaporator to enter a condenser, discharging the concentrated solution evaporated by the evaporator after the sulfuric acid content reaches more than 30%, and then further concentrating the concentrated solution into concentrated sulfuric acid with the content of more than 98% to be used as other industrial raw materials;
s03, cooling the water vapor and the hydrogen chloride gas which enter the condenser in the condenser, wherein water generated by the water vapor cooled by the condenser absorbs part of the hydrogen chloride gas to form dilute hydrochloric acid;
s04, allowing the cooled hydrogen chloride gas and the formed diluted hydrochloric acid to enter a hydrochloric acid absorption tower for absorption, and continuously extracting the absorbed hydrochloric acid after the absorbed hydrochloric acid is qualified, wherein the mass ratio of the feed hydrochloric acid to the extracted hydrochloric acid in the step S01 is controlled at 1:0.94-0.96.
2. The method for purifying hydrochloric acid containing sulfuric acid impurity according to claim 1, characterized by: the evaporator is heated by steam and is connected with a feed pump, a liquid flowmeter and a control valve.
3. The method for purifying hydrochloric acid containing sulfuric acid impurity according to claim 1, characterized by: the evaporator is also provided with an on-line measuring device and a sight glass.
4. The method for purifying hydrochloric acid containing sulfuric acid impurity according to claim 1, characterized by: and a gas flowmeter and a control valve are further arranged on the feeding pipeline of the condenser.
5. The method for purifying hydrochloric acid containing sulfuric acid impurity according to claim 1, characterized by: the hydrochloric acid absorption tower adopts two-stage absorption, and comprises a first-stage absorption tower and a second-stage absorption tower, wherein a gas phase outlet at the top end of the first-stage absorption tower is connected with the second-stage absorption tower, a gas phase outlet of the second-stage absorption tower is connected with a hydrogen chloride gas measuring device, and hydrochloric acid absorbed by the second-stage absorption tower is continuously extracted after being qualified.
6. The method for purifying hydrochloric acid containing sulfuric acid impurity according to claim 1, characterized by: the hydrochloric acid absorption tower is provided with a forced circulation pump for circulating the dilute hydrochloric acid in the tower kettle between the tower body and the tower kettle.
7. The method for purifying hydrochloric acid containing sulfuric acid impurity according to claim 1, characterized by: the hydrochloric acid absorption tower is provided with an acidity measuring device.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4222997A (en) * 1979-03-09 1980-09-16 Voss Steel Corporation Method of recovering hydrochloric acid from spent hydrochloric acid pickle waste
JPH05132302A (en) * 1991-11-08 1993-05-28 Denki Kagaku Kogyo Kk Method for purifying hydrogen chloride gas
CN1951801A (en) * 2006-06-15 2007-04-25 浙江工业大学 Process for preparing high purity hydrochloric acid by circularly absorbing hydrogen chloride by-product
CN105084315A (en) * 2015-07-29 2015-11-25 河南红东方化工股份有限公司 Method for recovering hydrochloric acid in chloroacetic acid production
CN105461138A (en) * 2015-12-28 2016-04-06 中南大学 Method for recycling sulfuric acid and hydrochloric acid from smelting wastewater and realizing fluorine open circuit
CN211496943U (en) * 2020-01-03 2020-09-15 重庆川维石化工程有限责任公司 Sulfuric acid and hydrochloric acid separation system

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4222997A (en) * 1979-03-09 1980-09-16 Voss Steel Corporation Method of recovering hydrochloric acid from spent hydrochloric acid pickle waste
JPH05132302A (en) * 1991-11-08 1993-05-28 Denki Kagaku Kogyo Kk Method for purifying hydrogen chloride gas
CN1951801A (en) * 2006-06-15 2007-04-25 浙江工业大学 Process for preparing high purity hydrochloric acid by circularly absorbing hydrogen chloride by-product
CN105084315A (en) * 2015-07-29 2015-11-25 河南红东方化工股份有限公司 Method for recovering hydrochloric acid in chloroacetic acid production
CN105461138A (en) * 2015-12-28 2016-04-06 中南大学 Method for recycling sulfuric acid and hydrochloric acid from smelting wastewater and realizing fluorine open circuit
CN211496943U (en) * 2020-01-03 2020-09-15 重庆川维石化工程有限责任公司 Sulfuric acid and hydrochloric acid separation system

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