CN110510579A - A device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid - Google Patents
A device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid Download PDFInfo
- Publication number
- CN110510579A CN110510579A CN201910635015.8A CN201910635015A CN110510579A CN 110510579 A CN110510579 A CN 110510579A CN 201910635015 A CN201910635015 A CN 201910635015A CN 110510579 A CN110510579 A CN 110510579A
- Authority
- CN
- China
- Prior art keywords
- separator
- hydrochloric acid
- hydrogen chloride
- pump
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
- C01B7/0737—Purification ; Separation of hydrogen chloride by extraction hydrogen chloride being extracted
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
本发明所述的一种从盐酸中解析分离氯化氢和水的装置及工艺，属于盐酸解析生产氯化氢的技术领域，包括盐酸解析系统、中和系统和浓缩系统，采用盐酸脱析法工艺生产氯化氢，具有纯度高(纯度>99.9％)和纯度波动小的优点，有利于氢氯化反应的自控，还能综合利用有机氯产品生产过程中低浓度的副产氯化氢，以制得高纯度的氯化氢气体，此外，产品氯化氢可借解析出的氯化氢的压力输送，从而省去氯化氢的加压设备，设备投资省，运行费用低，坏境污染少。
A device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid according to the present invention belongs to the technical field of producing hydrogen chloride by analyzing hydrochloric acid, including a hydrochloric acid analysis system, a neutralization system and a concentration system, and adopts a hydrochloric acid separation process to produce hydrogen chloride. It has the advantages of high purity (purity>99.9%) and small fluctuations in purity, which is beneficial to the self-control of hydrochlorination reaction, and can also comprehensively utilize low-concentration by-product hydrogen chloride in the production process of organic chlorine products to produce high-purity hydrogen chloride gas , In addition, the product hydrogen chloride can be transported by the pressure of the separated hydrogen chloride, thereby eliminating the pressure equipment for hydrogen chloride, saving equipment investment, low operating costs, and less environmental pollution.
Description
技术领域technical field
本发明涉及盐酸解析生产氯化氢的技术领域，具体涉及一种从盐酸中解析分离氯化氢和水的装置及工艺。The invention relates to the technical field of hydrochloric acid analysis to produce hydrogen chloride, in particular to a device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid.
背景技术Background technique
目前，应用比较成熟的稀盐酸脱析工艺主要有硫酸萃取精馏法、氯化钙萃取精馏法和变压精馏法(压差法)三种。At present, there are three kinds of mature dilute hydrochloric acid separation processes: sulfuric acid extractive distillation, calcium chloride extractive distillation and pressure swing rectification (differential pressure method).
硫酸萃取精馏法，该工艺的基本原理是利用硫酸与水完全互溶且较浓的硫酸沸点高于恒沸盐酸的沸点，使稀盐酸中的水转移到浓硫酸中形成相对较稀的硫酸，从而把氯化氢提出来，较稀的硫酸经蒸发脱水，浓缩为浓硫酸循环使用，蒸发出的水冷凝以后即为酸性废水。但使用的浓硫酸浓度要高，硫酸浓缩到浓硫酸时，沸点升高，该方法对设备要求较高，投资大，蒸发出的废水中含有氯化氢，不能达标排放。Sulfuric acid extraction and rectification method, the basic principle of this process is to use sulfuric acid to be completely miscible with water and the boiling point of denser sulfuric acid is higher than that of azeotropic hydrochloric acid, so that the water in dilute hydrochloric acid is transferred to concentrated sulfuric acid to form relatively dilute sulfuric acid. Hydrogen chloride is extracted, and the dilute sulfuric acid is evaporated and dehydrated, concentrated into concentrated sulfuric acid for recycling, and the evaporated water is condensed to become acidic wastewater. However, the concentration of concentrated sulfuric acid used should be high. When the sulfuric acid is concentrated to concentrated sulfuric acid, the boiling point will rise. This method requires high equipment and requires a large investment. The evaporated wastewater contains hydrogen chloride and cannot be discharged up to the standard.
氯化钙萃取精馏法，即在稀盐酸中加入氯化钙打破其共沸点的限制，把氯化氢分离出来。该方法采用高塔(填料塔)进行传质和传热，设备投资大，再沸器是利用虹吸的原理，循环速度慢，热效率低，氯化钙物料孔易结垢，设备寿命短，蒸发脱水为单效蒸发，热能利用低，蒸汽消耗高，废水中HCl浓度实际值在2-3％，蒸发装置采用石墨设备，投资大。Calcium chloride extractive distillation method, that is, adding calcium chloride to dilute hydrochloric acid to break the limitation of its azeotropic point, and separate hydrogen chloride. This method uses a high tower (packed tower) for mass transfer and heat transfer, and the equipment investment is large. The reboiler uses the principle of siphon, the circulation speed is slow, the thermal efficiency is low, the calcium chloride material hole is easy to scale, the equipment life is short, and the evaporation The dehydration is a single-effect evaporation, with low heat energy utilization and high steam consumption. The actual value of HCl concentration in the wastewater is 2-3%. The evaporation device adopts graphite equipment, which requires a large investment.
变压精馏法，基本原理是利用恒沸盐酸组成随压力而变化，相对于H2O和HCl，恒沸盐酸始终是高沸点组分的特点，从而达到使H2O和HCl分离的目的。该方法的主要设备为加压塔和负压塔，负压塔塔径大，塔高度高，设备投资大；塔顶回流，造成蒸气消耗大，即运行费用高。由于加压塔和负压塔之间物料的循环，操作要求严格，自动化水平要求高。The basic principle of the pressure swing distillation method is to use the composition of azeotropic hydrochloric acid to change with the pressure. Compared with H2O and HCl, azeotropic hydrochloric acid is always the characteristic of high boiling point components, so as to achieve the purpose of separating H2O and HCl . The main equipment of this method is a pressurized tower and a negative pressure tower. The negative pressure tower has a large diameter, a high tower height, and a large equipment investment; the reflux at the top of the tower causes large steam consumption, that is, high operating costs. Due to the circulation of materials between the pressure tower and the negative pressure tower, the operation requirements are strict and the automation level is high.
发明内容Contents of the invention
本发明提供一种从盐酸中解析分离氯化氢和水的装置及工艺，旨在解决现有设备及工艺投资大、运行成本高，有环境污染的问题。The invention provides a device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid, aiming at solving the problems of large investment, high operating cost and environmental pollution in the existing equipment and process.
本发明为解决上述技术问题，采用以下技术方案来实现：In order to solve the problems of the technologies described above, the present invention adopts the following technical solutions to realize:
一种从盐酸中解析分离氯化氢和水的装置，包括盐酸解析系统、中和系统和浓缩系统，所述的盐酸解析系统包括盐酸预热器、混合加热器、分离器、一级冷却器、二级冷却器、气液分离器、降膜蒸发分离器、闪蒸冷凝器、解析系统真空机组、解析系统液封槽；所述的中和系统包括氢氧化钙贮槽、螺旋计量秤、混合泵、缓冲罐、出料泵、过滤器；所述的浓缩系统包括一效蒸发分离器、二效蒸发分离器、氯化钙循环泵、蒸发冷凝器、浓缩系统真空机组、浓缩系统液封槽、废水泵；A device for analyzing and separating hydrogen chloride and water from hydrochloric acid, including a hydrochloric acid analysis system, a neutralization system, and a concentration system. The hydrochloric acid analysis system includes a hydrochloric acid preheater, a mixing heater, a separator, a primary cooler, and a secondary stage cooler, gas-liquid separator, falling film evaporation separator, flash condenser, analysis system vacuum unit, analysis system liquid seal tank; the neutralization system includes calcium hydroxide storage tank, screw weighing scale, mixing pump , a buffer tank, a discharge pump, a filter; the concentration system includes a first-effect evaporative separator, a second-effect evaporative separator, a calcium chloride circulation pump, an evaporative condenser, a concentration system vacuum unit, a concentration system liquid seal tank, waste water pump;
所述盐酸预热器底部加入盐酸溶液，中部加入蒸汽冷凝液，顶部出口连接混合加热器顶部入口，混合加热器中部通入蒸汽，底部出口连接分离器入口，分离器顶部出口连接一级冷却器，一级冷却器连接二级冷却器，二级冷却器连接气液分离器，气液分离器气相输出氯化氢气体，液相输出浓盐酸，分离器底部出口连接降膜蒸发分离器入口，降膜蒸发分离器中部通入蒸汽，气相出口连接闪蒸冷凝器，闪蒸冷凝器连接解析系统真空机组和解析系统液封槽，解析系统液封槽输出稀盐酸，降膜蒸发分离器的液相出口连接混合泵入口；Hydrochloric acid solution is added to the bottom of the hydrochloric acid preheater, steam condensate is added to the middle, the top outlet is connected to the top inlet of the mixing heater, steam is fed into the middle of the mixing heater, the bottom outlet is connected to the separator inlet, and the top outlet of the separator is connected to the primary cooler , the primary cooler is connected to the secondary cooler, and the secondary cooler is connected to the gas-liquid separator. The gas-liquid separator outputs hydrogen chloride gas in the gas phase, and the liquid phase outputs concentrated hydrochloric acid. The outlet at the bottom of the separator is connected to the inlet of the falling film evaporation separator, and the falling film Steam is introduced into the middle of the evaporation separator, the gas phase outlet is connected to the flash condenser, the flash condenser is connected to the vacuum unit of the analysis system and the liquid seal tank of the analysis system, the liquid seal tank of the analysis system outputs dilute hydrochloric acid, and the liquid phase outlet of the falling film evaporation separator Connect the mixing pump inlet;
所述氢氧化钙贮槽入口通入氢氧化钙，出口连接螺旋计量秤，螺旋计量秤连接混合泵，混合泵连接缓冲罐，缓冲罐连接出料泵，出料泵连接过滤器，过滤器连接一效蒸发分离器入口，同时过滤出氯化钙；The inlet of the calcium hydroxide storage tank is fed with calcium hydroxide, the outlet is connected to the screw weighing scale, the screw weighing scale is connected to the mixing pump, the mixing pump is connected to the buffer tank, the buffer tank is connected to the discharge pump, the discharge pump is connected to the filter, and the filter is connected to the At the inlet of the first-effect evaporation separator, calcium chloride is filtered out at the same time;
所述一效蒸发分离器气相出口连接蒸发冷凝器，蒸发冷凝器连接浓缩系统真空机组和浓缩系统液封槽，浓缩系统液封槽连接废水泵，废水泵输出水，一效蒸发分离器液相出口部分连接浓缩系统液封槽，部分连接二效蒸发分离器，二效蒸发分离器中部通入蒸汽，二效蒸发分离器气相出口连接一效蒸发分离器，液相出口连接氯化钙循环泵，氯化钙循环泵连接混合加热器入口。The gas phase outlet of the first-effect evaporative separator is connected to the evaporative condenser, the evaporative condenser is connected to the vacuum unit of the concentration system and the liquid seal tank of the concentration system, the liquid seal tank of the concentration system is connected to the waste water pump, and the waste water pump outputs water, and the liquid phase of the first effect evaporative separator The outlet part is connected to the liquid-sealed tank of the concentration system, partly connected to the second-effect evaporator separator, the middle part of the second-effect evaporator separator is fed with steam, the gas phase outlet of the second-effect evaporator separator is connected to the first-effect evaporator separator, and the liquid phase outlet is connected to the calcium chloride circulation pump , the calcium chloride circulation pump is connected to the mixing heater inlet.
作为优选，所述的二级冷却器底部输出浓盐酸。As a preference, the bottom of the secondary cooler outputs concentrated hydrochloric acid.
作为优选，所述盐酸预热器的盐酸溶液入口设有盐酸泵和流量计。Preferably, the hydrochloric acid solution inlet of the hydrochloric acid preheater is provided with a hydrochloric acid pump and a flow meter.
基于上述装置的一种连续生产氯乙酸的工艺，包含以下步骤：A kind of technique of continuous production of chloroacetic acid based on above-mentioned device, comprises the following steps:
(1)盐酸溶液经盐酸泵、流量计送入盐酸预热器并通入蒸汽冷凝液预热后送入混合加热器；(1) The hydrochloric acid solution is sent into the hydrochloric acid preheater through the hydrochloric acid pump and flowmeter, and then fed into the steam condensate for preheating and then sent into the mixing heater;
(2)送入混合加热器的盐酸溶液与来自氯化钙循环泵的浓度为55-60％的氯化钙溶液充分混合并通入蒸汽调节温度后送入分离器；(2) the hydrochloric acid solution sent into the mixing heater is fully mixed with the calcium chloride solution of 55-60% from the concentration of the calcium chloride circulation pump and fed into the separator after steam regulation temperature;
(3)在分离器内解析出氯化氢气体从顶部出口排出并依次经过一级冷却器、二级冷却器、气液分离器后进入下工序，二级冷却器和气液分离器中的浓盐酸送入浓盐酸贮槽；分离器底部的稀氯化钙溶液进入降膜蒸发分离器；(3) Analyze the hydrogen chloride gas in the separator and discharge it from the top outlet and enter the next process after passing through the primary cooler, the secondary cooler, and the gas-liquid separator successively. The concentrated hydrochloric acid in the secondary cooler and the gas-liquid separator is sent to into the concentrated hydrochloric acid storage tank; the dilute calcium chloride solution at the bottom of the separator enters the falling film evaporation separator;
(4)降膜蒸发分离器的气相进入闪蒸冷凝器将氯化钙中的氯化氢进一步脱出，冷凝后的稀盐酸溶液进入解析系统液封槽后送入稀盐酸贮槽，闪蒸冷凝器中的不凝性气体进入解析系统真空机组，降膜蒸发分离器的液相与来自氢氧化钙贮槽的氢氧化钙在混合泵入口泵动混合并调节PH值为7-7.5后进入缓冲罐，再经过出料泵加压和过滤器过滤后进入一效蒸发分离器，过滤器过滤出氯化钙；(4) The gas phase of the falling film evaporation separator enters the flash condenser to further remove the hydrogen chloride in the calcium chloride, and the condensed dilute hydrochloric acid solution enters the liquid seal tank of the analysis system and then is sent to the dilute hydrochloric acid storage tank and the flash condenser The non-condensable gas enters the vacuum unit of the analysis system, and the liquid phase of the falling film evaporation separator and the calcium hydroxide from the calcium hydroxide storage tank are pumped and mixed at the inlet of the mixing pump and adjusted to a pH value of 7-7.5 before entering the buffer tank. After being pressurized by the discharge pump and filtered by the filter, it enters the first-effect evaporation separator, and the filter filters out calcium chloride;
(5)一效蒸发分离器的气相进入蒸发冷凝器冷却后进入浓缩系统液封槽，在浓缩系统液封槽中与部分液相混合后由废水泵排出，蒸发冷凝器中的不凝性气体进入浓缩系统真空机组，一效蒸发分离器的部分液相进入二效蒸发分离器；(5) The gas phase of the first-effect evaporative separator enters the evaporative condenser to cool and then enters the liquid seal tank of the concentration system. After being mixed with part of the liquid phase in the liquid seal tank of the concentration system, it is discharged by the waste water pump. The non-condensable gas in the evaporative condenser Enter the vacuum unit of the concentration system, and part of the liquid phase of the first-effect evaporator separator enters the second-effect evaporator separator;
(6)二效蒸发分离器的气相进入一效蒸发分离器，液相经氯化钙循环泵送入混合加热器；(6) The gas phase of the second-effect evaporation separator enters the first-effect evaporation separator, and the liquid phase is sent into the mixing heater through the calcium chloride circulation pump;
作为优选，所述步骤(1)的预热温度为70-80℃。As a preference, the preheating temperature of the step (1) is 70-80°C.
作为优选，所述步骤(2)中混合加热器通入蒸汽调节溶液温度为115-125℃。As a preference, in the step (2), the mixing heater feeds steam to adjust the temperature of the solution to 115-125°C.
作为优选，所述步骤(4)中降膜蒸发分离器通入蒸汽调节溶液温度为120-130℃，使液相氯化钙溶液中氯化氢含量降低至0.3％以下。As preferably, in the step (4), the falling film evaporation separator feeds steam to adjust the temperature of the solution to 120-130° C., so that the hydrogen chloride content in the liquid-phase calcium chloride solution is reduced to below 0.3%.
作为优选，所述步骤(6)中二效蒸发分离器通入蒸汽调节溶液温度为120-130℃。As a preference, in the step (6), the second-effect evaporation separator is fed with steam to adjust the temperature of the solution to 120-130°C.
与现有技术相比，本发明的有益效果是：Compared with prior art, the beneficial effect of the present invention is:
1、设备投资省：由于采用了压力较高的盐酸与高浓度的氯化钙的充分混合，在混合加热器物料管内设置了微分混合结构，盐酸与高浓度的氯化钙的充分混合，省去了高大的石墨解析塔及填料；采用稀氯化钙溶液真空降膜蒸发将稀氯化钙中的氯化氢进一步降低，为中和过程减少了氢氧化钙的用量，并经中和的氯化钙溶液成为碱性，在氯化钙浓缩时也可降低对设备材质的要求，节省了设备投资。1. Low equipment investment: Due to the full mixing of high-pressure hydrochloric acid and high-concentration calcium chloride, a differential mixing structure is set in the material tube of the mixing heater, and the full mixing of hydrochloric acid and high-concentration calcium chloride saves The tall graphite analysis tower and packing were removed; the hydrogen chloride in the dilute calcium chloride was further reduced by vacuum falling film evaporation of dilute calcium chloride solution, which reduced the amount of calcium hydroxide used in the neutralization process, and the neutralized chloride The calcium solution becomes alkaline, which can also reduce the requirements for equipment materials when the calcium chloride is concentrated, saving equipment investment.
2、运行费用低：由于取消了解析塔，盐酸与氯化钙混合液以雾化的方式进入分离器，其分离器就是一个空的容器，并且解析温度在115-125℃，比解析塔运行时塔底温度低20度之多，可节约能耗；采用中和含酸氯化钙的方法，氯化钙浓缩可选用二效蒸发，蒸汽得到了二次利用，蒸汽消耗大大的减少，这也是该发明的核心所在；取消了再沸器，可避免设备的结垢，保障了设备的长久运行，省去了设备的更新费用。采用了二次解析氯化氢的方式(第一次加压解析，第二次真空解析)氯化氢利用率提高，稀氯化钙中氯化氢含量大大降低，也减少了氢氧化钙用量，降低了采购成本。2. Low operating cost: due to the cancellation of the desorption tower, the mixture of hydrochloric acid and calcium chloride enters the separator in the form of atomization, and the separator is an empty container, and the desorption temperature is 115-125 ° C, which is better than the desorption tower. When the temperature at the bottom of the tower is as low as 20 degrees, energy consumption can be saved; the method of neutralizing acid-containing calcium chloride is adopted, and the second-effect evaporation can be used for calcium chloride concentration, and the steam is used twice, and the steam consumption is greatly reduced. It is also the core of the invention; the reboiler is cancelled, which can avoid scaling of the equipment, guarantee the long-term operation of the equipment, and save the renewal cost of the equipment. The second analysis of hydrogen chloride is adopted (the first pressure analysis, the second vacuum analysis). The utilization rate of hydrogen chloride is improved, the content of hydrogen chloride in dilute calcium chloride is greatly reduced, the amount of calcium hydroxide is also reduced, and the purchase cost is reduced.
3、清洁化生产：由于采用了中和的方式解决了氯化钙中氯化氢转化为氯化钙，使分离出的水达到无氯化氢排放。这部分水可以进行中水回用，或用反渗透膜处理，生产纯水。氯化氢经中和反应过程中多余的量能不断的排出，是进行了不断的置换与更新，在系统中设置了过滤器不仅过滤氢氧化钙反应产生的杂质，也可滤除系统中其它杂质，避免了解析塔工艺中定期置换氯化钙带来的氯化钙溶液处理的环保问题。3. Clean production: Due to the neutralization method, the hydrogen chloride in the calcium chloride is converted into calcium chloride, so that the separated water can achieve no hydrogen chloride discharge. This part of water can be reused as reclaimed water or treated with reverse osmosis membrane to produce pure water. The excess amount of hydrogen chloride can be continuously discharged during the neutralization reaction, which is a continuous replacement and renewal. The filter is installed in the system not only to filter the impurities produced by the calcium hydroxide reaction, but also to filter out other impurities in the system. The environmental protection problem of calcium chloride solution treatment caused by regular replacement of calcium chloride in the analytical tower process is avoided.
附图说明Description of drawings
附图用来提供对本发明的进一步理解，并且构成说明书的一部分，与本发明的实施例一起用于解释本发明，并不构成对本发明的限制。在附图中：The accompanying drawings are used to provide a further understanding of the present invention, and constitute a part of the description, and are used together with the embodiments of the present invention to explain the present invention, and do not constitute a limitation to the present invention. In the attached picture:
图1为本发明的流程图。Fig. 1 is a flowchart of the present invention.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
如图所示：一种从盐酸中解析分离氯化氢和水的装置，包括盐酸解析系统、中和系统和浓缩系统，所述的盐酸解析系统包括盐酸预热器101、混合加热器102、分离器103、一级冷却器104、二级冷却器105、气液分离器106、降膜蒸发分离器107、闪蒸冷凝器108、解析系统真空机组109、解析系统液封槽110；所述的中和系统包括氢氧化钙贮槽201、螺旋计量秤202、混合泵203、缓冲罐204、出料泵205、过滤器206；所述的浓缩系统包括一效蒸发分离器301、二效蒸发分离器302、氯化钙循环泵303、蒸发冷凝器304、浓缩系统真空机组305、浓缩系统液封槽306、废水泵307；As shown in the figure: a device for analyzing and separating hydrogen chloride and water from hydrochloric acid, including a hydrochloric acid analysis system, a neutralization system, and a concentration system. The hydrochloric acid analysis system includes a hydrochloric acid preheater 101, a mixing heater 102, and a separator 103, primary cooler 104, secondary cooler 105, gas-liquid separator 106, falling film evaporation separator 107, flash condenser 108, analysis system vacuum unit 109, analysis system liquid seal tank 110; And system comprises calcium hydroxide storage tank 201, screw metering scale 202, mixing pump 203, buffer tank 204, discharge pump 205, filter 206; Described concentration system comprises one effect evaporation separator 301, two effect evaporation separator 302, calcium chloride circulating pump 303, evaporative condenser 304, concentration system vacuum unit 305, concentration system liquid seal tank 306, waste water pump 307;
所述盐酸预热器101底部加入盐酸溶液，盐酸预热器101的盐酸溶液入口设有盐酸泵和流量计，中部加入蒸汽冷凝液，顶部出口连接混合加热器102顶部入口，混合加热器102中部通入蒸汽，底部出口连接分离器103入口，分离器103顶部出口连接一级冷却器104，一级冷却器104连接二级冷却器105，二级冷却器105连接气液分离器106，气液分离器106气相输出氯化氢气体，液相和二级冷却器105底部输出浓盐酸，分离器103底部出口连接降膜蒸发分离器107入口，降膜蒸发分离器107中部通入蒸汽，气相出口连接闪蒸冷凝器108，闪蒸冷凝器108连接解析系统真空机组109和解析系统液封槽110，解析系统液封槽110输出稀盐酸，降膜蒸发分离器107的液相出口连接混合泵203入口；The hydrochloric acid solution is added to the bottom of the hydrochloric acid preheater 101, the hydrochloric acid solution inlet of the hydrochloric acid preheater 101 is provided with a hydrochloric acid pump and a flow meter, and steam condensate is added to the middle part, and the top outlet is connected to the top inlet of the mixing heater 102, and the middle part of the mixing heater 102 Steam is introduced, the bottom outlet is connected to the inlet of the separator 103, the top outlet of the separator 103 is connected to the primary cooler 104, the primary cooler 104 is connected to the secondary cooler 105, the secondary cooler 105 is connected to the gas-liquid separator 106, and the gas-liquid The separator 106 outputs hydrogen chloride gas in the gas phase, the liquid phase and the bottom of the secondary cooler 105 output concentrated hydrochloric acid, the outlet at the bottom of the separator 103 is connected to the inlet of the falling film evaporation separator 107, the middle part of the falling film evaporation separator 107 is fed with steam, and the outlet of the gas phase is connected to the flash The evaporation condenser 108 and the flash condenser 108 are connected to the analysis system vacuum unit 109 and the analysis system liquid seal tank 110, the analysis system liquid seal tank 110 outputs dilute hydrochloric acid, and the liquid phase outlet of the falling film evaporation separator 107 is connected to the inlet of the mixing pump 203;
所述氢氧化钙贮槽201入口通入氢氧化钙，出口连接螺旋计量秤202，螺旋计量秤202连接混合泵203，混合泵203连接缓冲罐204，缓冲罐204连接出料泵205，出料泵205连接过滤器206，过滤器206连接一效蒸发分离器301入口，同时过滤出氯化钙；The entrance of the calcium hydroxide storage tank 201 is fed with calcium hydroxide, the outlet is connected to the screw weighing scale 202, the screw weighing scale 202 is connected to the mixing pump 203, the mixing pump 203 is connected to the buffer tank 204, and the buffer tank 204 is connected to the discharge pump 205, and the discharge The pump 205 is connected to the filter 206, and the filter 206 is connected to the inlet of the first-effect evaporative separator 301, and calcium chloride is filtered out simultaneously;
所述一效蒸发分离器301气相出口连接蒸发冷凝器304，蒸发冷凝器304连接浓缩系统真空机组305和浓缩系统液封槽306，浓缩系统液封槽306连接废水泵307，废水泵307输出水，一效蒸发分离器301液相出口部分连接浓缩系统液封槽306，部分连接二效蒸发分离器302，二效蒸发分离器302中部通入蒸汽，二效蒸发分离器302气相出口连接一效蒸发分离器301，液相出口连接氯化钙循环泵303，氯化钙循环泵303连接混合加热器102入口。The gas phase outlet of the one-effect evaporative separator 301 is connected to the evaporative condenser 304, the evaporative condenser 304 is connected to the concentration system vacuum unit 305 and the concentration system liquid seal tank 306, the concentration system liquid seal tank 306 is connected to the waste water pump 307, and the waste water pump 307 outputs water , the liquid phase outlet of the first effect evaporator separator 301 is partly connected to the liquid seal tank 306 of the concentration system, partly connected to the second effect evaporator separator 302, the middle part of the second effect evaporator separator 302 is fed with steam, and the gas phase outlet of the second effect evaporator separator 302 is connected to the first effect Evaporation separator 301, the outlet of liquid phase is connected to calcium chloride circulation pump 303, and calcium chloride circulation pump 303 is connected to the inlet of mixing heater 102.
实施例1：Example 1:
(1)盐酸溶液经盐酸泵、流量计送入盐酸预热器并通入蒸汽冷凝液预热到70℃后送入混合加热器；(1) The hydrochloric acid solution is sent to the hydrochloric acid preheater through the hydrochloric acid pump and flow meter, and the steam condensate is fed into the preheater to 70°C before being sent to the mixing heater;
(2)送入混合加热器的盐酸溶液与来自氯化钙循环泵的浓度为55-60％的氯化钙溶液充分混合并通入蒸汽调节温度为115℃后送入分离器；(2) the hydrochloric acid solution sent into the mixed heater is fully mixed with the calcium chloride solution of 55-60% from the concentration of the calcium chloride circulating pump and feeds into the separator after steam regulation temperature is 115°C;
(3)在分离器内解析出氯化氢气体从顶部出口排出并依次经过一级冷却器、二级冷却器、气液分离器后进入下工序，二级冷却器和气液分离器中的浓盐酸送入浓盐酸贮槽；分离器底部的稀氯化钙溶液进入降膜蒸发分离器；(3) Analyze the hydrogen chloride gas in the separator and discharge it from the top outlet and enter the next process after passing through the primary cooler, the secondary cooler, and the gas-liquid separator successively. The concentrated hydrochloric acid in the secondary cooler and the gas-liquid separator is sent to into the concentrated hydrochloric acid storage tank; the dilute calcium chloride solution at the bottom of the separator enters the falling film evaporation separator;
(4)降膜蒸发分离器的气相进入闪蒸冷凝器将氯化钙中的氯化氢进一步脱出，冷凝后的稀盐酸溶液进入解析系统液封槽后送入稀盐酸贮槽，闪蒸冷凝器中的不凝性气体进入解析系统真空机组，调节降膜蒸发分离器内温度为120℃，降膜蒸发分离器的液相与来自氢氧化钙贮槽的氢氧化钙在混合泵入口泵动混合并调节PH值为7后进入缓冲罐，再经过出料泵加压和过滤器过滤后进入一效蒸发分离器，过滤器过滤出氯化钙；(4) The gas phase of the falling film evaporation separator enters the flash condenser to further remove the hydrogen chloride in the calcium chloride, and the condensed dilute hydrochloric acid solution enters the liquid seal tank of the analysis system and then is sent to the dilute hydrochloric acid storage tank and the flash condenser The non-condensable gas enters the vacuum unit of the analysis system, and the temperature in the falling film evaporation separator is adjusted to 120 ° C. The liquid phase of the falling film evaporation separator and the calcium hydroxide from the calcium hydroxide storage tank are pumped and mixed at the inlet of the mixing pump. After adjusting the pH value to 7, it enters the buffer tank, and then enters the first-effect evaporation separator after being pressurized by the discharge pump and filtered by the filter, and the filter filters out calcium chloride;
(5)一效蒸发分离器的气相进入蒸发冷凝器冷却后进入浓缩系统液封槽，在浓缩系统液封槽中与部分液相混合后由废水泵排出，蒸发冷凝器中的不凝性气体进入浓缩系统真空机组，一效蒸发分离器的部分液相进入二效蒸发分离器；(5) The gas phase of the first-effect evaporative separator enters the evaporative condenser to cool and then enters the liquid seal tank of the concentration system. After being mixed with part of the liquid phase in the liquid seal tank of the concentration system, it is discharged by the waste water pump. The non-condensable gas in the evaporative condenser Enter the vacuum unit of the concentration system, and part of the liquid phase of the first-effect evaporator separator enters the second-effect evaporator separator;
(6)调节二效蒸发分离器内温度为120℃，二效蒸发分离器的气相进入一效蒸发分离器，液相经氯化钙循环泵送入混合加热器。(6) Adjust the temperature in the second-effect evaporation separator to 120°C, the gas phase of the second-effect evaporation separator enters the first-effect evaporation separator, and the liquid phase is sent to the mixing heater through the calcium chloride circulation pump.
实施例2：Example 2:
(1)盐酸溶液经盐酸泵、流量计送入盐酸预热器并通入蒸汽冷凝液预热到80℃后送入混合加热器；(1) The hydrochloric acid solution is sent to the hydrochloric acid preheater through the hydrochloric acid pump and flow meter, and the steam condensate is fed into the preheater to 80°C before being sent to the mixing heater;
(2)送入混合加热器的盐酸溶液与来自氯化钙循环泵的浓度为55-60％的氯化钙溶液充分混合并通入蒸汽调节温度为125℃后送入分离器；(2) the hydrochloric acid solution sent into the mixing heater is fully mixed with the calcium chloride solution of 55-60% from the concentration of the calcium chloride circulation pump and feeds into the separator after steam regulation temperature is 125°C;
(3)在分离器内解析出氯化氢气体从顶部出口排出并依次经过一级冷却器、二级冷却器、气液分离器后进入下工序，二级冷却器和气液分离器中的浓盐酸送入浓盐酸贮槽；分离器底部的稀氯化钙溶液进入降膜蒸发分离器；(3) Analyze the hydrogen chloride gas in the separator and discharge it from the top outlet and enter the next process after passing through the primary cooler, the secondary cooler, and the gas-liquid separator successively. The concentrated hydrochloric acid in the secondary cooler and the gas-liquid separator is sent to into the concentrated hydrochloric acid storage tank; the dilute calcium chloride solution at the bottom of the separator enters the falling film evaporation separator;
(4)降膜蒸发分离器的气相进入闪蒸冷凝器将氯化钙中的氯化氢进一步脱出，冷凝后的稀盐酸溶液进入解析系统液封槽后送入稀盐酸贮槽，闪蒸冷凝器中的不凝性气体进入解析系统真空机组，调节降膜蒸发分离器内温度为130℃，降膜蒸发分离器的液相与来自氢氧化钙贮槽的氢氧化钙在混合泵入口泵动混合并调节PH值为7.5后进入缓冲罐，再经过出料泵加压和过滤器过滤后进入一效蒸发分离器，过滤器过滤出氯化钙；(4) The gas phase of the falling film evaporation separator enters the flash condenser to further remove the hydrogen chloride in the calcium chloride, and the condensed dilute hydrochloric acid solution enters the liquid seal tank of the analysis system and then is sent to the dilute hydrochloric acid storage tank and the flash condenser The non-condensable gas enters the vacuum unit of the analysis system, and the temperature in the falling film evaporation separator is adjusted to 130 ° C. The liquid phase of the falling film evaporation separator and the calcium hydroxide from the calcium hydroxide storage tank are pumped and mixed at the inlet of the mixing pump. After adjusting the pH value to 7.5, it enters the buffer tank, and then enters the first-effect evaporation separator after being pressurized by the discharge pump and filtered by the filter, and the filter filters out calcium chloride;
(5)一效蒸发分离器的气相进入蒸发冷凝器冷却后进入浓缩系统液封槽，在浓缩系统液封槽中与部分液相混合后由废水泵排出，蒸发冷凝器中的不凝性气体进入浓缩系统真空机组，一效蒸发分离器的部分液相进入二效蒸发分离器；(5) The gas phase of the first-effect evaporative separator enters the evaporative condenser to cool and then enters the liquid seal tank of the concentration system. After being mixed with part of the liquid phase in the liquid seal tank of the concentration system, it is discharged by the waste water pump. The non-condensable gas in the evaporative condenser Enter the vacuum unit of the concentration system, and part of the liquid phase of the first-effect evaporator separator enters the second-effect evaporator separator;
(6)调节二效蒸发分离器内温度为130℃，二效蒸发分离器的气相进入一效蒸发分离器，液相经氯化钙循环泵送入混合加热器。(6) Adjust the temperature in the second-effect evaporation separator to 130°C, the gas phase of the second-effect evaporation separator enters the first-effect evaporation separator, and the liquid phase is sent to the mixing heater through a calcium chloride circulation pump.
实施例3：Example 3:
(1)盐酸溶液经盐酸泵、流量计送入盐酸预热器并通入蒸汽冷凝液预热到75℃后送入混合加热器；(1) The hydrochloric acid solution is sent to the hydrochloric acid preheater through the hydrochloric acid pump and flow meter, and the steam condensate is fed into the preheated to 75°C before being sent to the mixing heater;
(2)送入混合加热器的盐酸溶液与来自氯化钙循环泵的浓度为55-60％的氯化钙溶液充分混合并通入蒸汽调节温度为120℃后送入分离器；(2) the hydrochloric acid solution sent into the mixed heater is fully mixed with the calcium chloride solution of 55-60% from the concentration of the calcium chloride circulation pump and fed into the steam to adjust the temperature to be sent to the separator after 120°C;
(3)在分离器内解析出氯化氢气体从顶部出口排出并依次经过一级冷却器、二级冷却器、气液分离器后进入下工序，二级冷却器和气液分离器中的浓盐酸送入浓盐酸贮槽；分离器底部的稀氯化钙溶液进入降膜蒸发分离器；(3) Analyze the hydrogen chloride gas in the separator and discharge it from the top outlet and enter the next process after passing through the primary cooler, the secondary cooler, and the gas-liquid separator successively. The concentrated hydrochloric acid in the secondary cooler and the gas-liquid separator is sent to into the concentrated hydrochloric acid storage tank; the dilute calcium chloride solution at the bottom of the separator enters the falling film evaporation separator;
(4)降膜蒸发分离器的气相进入闪蒸冷凝器将氯化钙中的氯化氢进一步脱出，冷凝后的稀盐酸溶液进入解析系统液封槽后送入稀盐酸贮槽，闪蒸冷凝器中的不凝性气体进入解析系统真空机组，调节降膜蒸发分离器内温度为125℃，降膜蒸发分离器的液相与来自氢氧化钙贮槽的氢氧化钙在混合泵入口泵动混合并调节PH值为7.2后进入缓冲罐，再经过出料泵加压和过滤器过滤后进入一效蒸发分离器，过滤器过滤出氯化钙；(4) The gas phase of the falling film evaporation separator enters the flash condenser to further remove the hydrogen chloride in the calcium chloride, and the condensed dilute hydrochloric acid solution enters the liquid seal tank of the analysis system and then is sent to the dilute hydrochloric acid storage tank and the flash condenser The non-condensable gas enters the vacuum unit of the analysis system, and the temperature in the falling film evaporation separator is adjusted to 125 ° C. The liquid phase of the falling film evaporation separator and the calcium hydroxide from the calcium hydroxide storage tank are pumped and mixed at the inlet of the mixing pump. After adjusting the pH value to 7.2, it enters the buffer tank, and then enters the first-effect evaporation separator after being pressurized by the discharge pump and filtered by the filter, and the filter filters out calcium chloride;
(5)一效蒸发分离器的气相进入蒸发冷凝器冷却后进入浓缩系统液封槽，在浓缩系统液封槽中与部分液相混合后由废水泵排出，蒸发冷凝器中的不凝性气体进入浓缩系统真空机组，一效蒸发分离器的部分液相进入二效蒸发分离器；(5) The gas phase of the first-effect evaporative separator enters the evaporative condenser to cool and then enters the liquid seal tank of the concentration system. After being mixed with part of the liquid phase in the liquid seal tank of the concentration system, it is discharged by the waste water pump. The non-condensable gas in the evaporative condenser Enter the vacuum unit of the concentration system, and part of the liquid phase of the first-effect evaporator separator enters the second-effect evaporator separator;
(6)调节二效蒸发分离器内温度为125℃，二效蒸发分离器的气相进入一效蒸发分离器，液相经氯化钙循环泵送入混合加热器。(6) Adjust the temperature in the second-effect evaporation separator to 125°C, the gas phase of the second-effect evaporation separator enters the first-effect evaporation separator, and the liquid phase is sent to the mixing heater through a calcium chloride circulation pump.
本方法步骤(3)中解析获得的氯化氢，具有纯度高(纯度>99.9％)和纯度波动小的优点，有利于氢氯化反应的自控。The hydrogen chloride obtained by analysis in step (3) of the method has the advantages of high purity (purity>99.9%) and small fluctuation of purity, and is beneficial to the self-control of hydrochlorination reaction.
以上仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。The above are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention. Inside.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910635015.8A CN110510579A (en) | 2019-07-15 | 2019-07-15 | A device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910635015.8A CN110510579A (en) | 2019-07-15 | 2019-07-15 | A device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110510579A true CN110510579A (en) | 2019-11-29 |
Family
ID=68623220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910635015.8A Pending CN110510579A (en) | 2019-07-15 | 2019-07-15 | A device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110510579A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110921630A (en) * | 2019-12-09 | 2020-03-27 | 北京诺维新材科技有限公司 | Method for preparing hydrogen chloride by resolving hydrochloric acid |
| CN116459636A (en) * | 2023-05-05 | 2023-07-21 | 南通星球石墨股份有限公司 | Deep-resolution hydrochloric acid treatment device |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB669671A (en) * | 1949-05-03 | 1952-04-09 | Wingfoot Corp | Production of gaseous hydrogen chloride from an aqueous solution thereof |
| CN101525121A (en) * | 2009-04-16 | 2009-09-09 | 张孟存 | Method for analyzing chlorine hydride in hydrochloric acid |
| CN108840310A (en) * | 2018-09-27 | 2018-11-20 | 淄博晟钛复合材料科技有限公司 | A kind of device and its technique of producing hydrogen chloride by resolving deep from dilute hydrochloric acid |
| CN109809361A (en) * | 2019-04-11 | 2019-05-28 | 常州安海化工工程技术有限公司 | A kind of de- analysis technique of the hydrochloric acid of high-efficiency environment friendly |
| CN210710735U (en) * | 2019-07-15 | 2020-06-09 | 杭州众立化工科技有限公司 | Device for resolving and separating hydrogen chloride and water from hydrochloric acid |
-
2019
- 2019-07-15 CN CN201910635015.8A patent/CN110510579A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB669671A (en) * | 1949-05-03 | 1952-04-09 | Wingfoot Corp | Production of gaseous hydrogen chloride from an aqueous solution thereof |
| CN101525121A (en) * | 2009-04-16 | 2009-09-09 | 张孟存 | Method for analyzing chlorine hydride in hydrochloric acid |
| CN108840310A (en) * | 2018-09-27 | 2018-11-20 | 淄博晟钛复合材料科技有限公司 | A kind of device and its technique of producing hydrogen chloride by resolving deep from dilute hydrochloric acid |
| CN109809361A (en) * | 2019-04-11 | 2019-05-28 | 常州安海化工工程技术有限公司 | A kind of de- analysis technique of the hydrochloric acid of high-efficiency environment friendly |
| CN210710735U (en) * | 2019-07-15 | 2020-06-09 | 杭州众立化工科技有限公司 | Device for resolving and separating hydrogen chloride and water from hydrochloric acid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110921630A (en) * | 2019-12-09 | 2020-03-27 | 北京诺维新材科技有限公司 | Method for preparing hydrogen chloride by resolving hydrochloric acid |
| CN116459636A (en) * | 2023-05-05 | 2023-07-21 | 南通星球石墨股份有限公司 | Deep-resolution hydrochloric acid treatment device |
| CN116459636B (en) * | 2023-05-05 | 2024-05-17 | 南通星球石墨股份有限公司 | Deep-resolution hydrochloric acid treatment device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN210683206U (en) | Waste acid treatment system | |
| CN111704109A (en) | Method and system for preparing electronic-grade hydrofluoric acid by continuous method | |
| CN106745062B (en) | A process and device for producing concentrated ammonia water by negative pressure operation | |
| CN108715456B (en) | Method for recycling electrode foil corrosion waste nitric acid | |
| CN105693585A (en) | System and method for separating N-methylpyrrolidone/chloroform | |
| WO2021129404A1 (en) | Device and method for recycling waste acid liquid for polycrystalline silicon texturing | |
| CN111330412B (en) | System and process for absorbing and purifying byproduct hydrogen chloride gas in chlorination section into acid | |
| CN208893656U (en) | A kind of equipment for NMP recovery heat pump rectification in lithium battery production | |
| CN106673012A (en) | A process and device for producing concentrated ammonia water by negative pressure operation | |
| CN110510579A (en) | A device and process for analyzing and separating hydrogen chloride and water from hydrochloric acid | |
| CN203683302U (en) | Evaporating device for wastewater with high content of salt | |
| CN210826001U (en) | O-chlorobenzonitrile production system | |
| CN210710735U (en) | Device for resolving and separating hydrogen chloride and water from hydrochloric acid | |
| CN110330418B (en) | Method for recovering formaldehyde gas volatilized in normal pressure device in pentaerythritol production | |
| CN205109056U (en) | Sour vapor removal recovery unit of red fuming nitric acid (RFNA) production | |
| CN104860269B (en) | The recovery method and device of hydrochloric acid in industrial wastes | |
| CN206476756U (en) | A device for producing concentrated ammonia water by negative pressure operation | |
| CN111943141A (en) | Hydrochloric acid analysis device with negative pressure dehydration function and analysis process | |
| CN206244421U (en) | A device for producing concentrated ammonia water by negative pressure operation | |
| CN106744720B (en) | The circulation recycling system and its operation process of trichloroacetaldehyde by-product dilute sulfuric acid | |
| CN204265453U (en) | A kind of device of lower concentration ammoniacal liquor high purity ammonia | |
| CN211338795U (en) | Hydrogen chloride production system | |
| CN104190100B (en) | Flow-reversing dual-purpose ammonia enrichment facility and application thereof | |
| CN211896157U (en) | Nitric acid wastewater treatment system containing aluminum nitrate | |
| CN208843875U (en) | A kind of high saliferous waste water treatment system containing solvent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191129 |
|
| RJ01 | Rejection of invention patent application after publication |