CN101691210B - Method for concentrating titanium white waste acid by utilizing sulfuric-acid production tail gas - Google Patents
Method for concentrating titanium white waste acid by utilizing sulfuric-acid production tail gas Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及工业废料的回收利用方法，特别是涉及一种利用硫酸生产尾气提浓钛白废酸的方法。The invention relates to a method for recycling industrial waste, in particular to a method for using sulfuric acid production tail gas to concentrate titanium dioxide waste acid.
背景技术Background technique
钛白废酸是钛白粉生产过程中产生的工业废料，每生产一吨钛白粉大约产生4～5吨钛白废酸。由于钛白废酸中的硫酸含量低(20％左右，以硫酸计质量百分比，下同)且含大量无机盐，无法将其直接回收利用。但是，如果提浓钛白废酸，使钛白废酸中的硫酸含量按质量百分比计达到55％以上时，其中的大部分无机盐就会析出，此时就可以将其回收利用。目前大多数钛白粉厂通常是采用蒸汽加热的方式，在反应釜或是蒸发器中将钛白废酸中的水份蒸发掉，这样提浓钛白废酸的效率虽然比较高，但是实际生产过程中会发生高温结垢、浓缩后的料浆堵塞换热器或管道等事故，严重影响工厂开车率，而且由于废酸浓缩是在高温下进行，对设备要求非常高，投资较大，运行和维修费用较高。Titanium dioxide waste acid is an industrial waste produced during the production of titanium dioxide, and about 4 to 5 tons of titanium dioxide waste acid is produced for every ton of titanium dioxide produced. Because the content of sulfuric acid in titanium dioxide waste acid is low (about 20%, the mass percent in sulfuric acid, the same below) and contains a large amount of inorganic salts, it cannot be directly recycled. However, if the spent titanium white acid is concentrated so that the sulfuric acid content in the spent titanium white acid reaches more than 55% by mass, most of the inorganic salts will be precipitated, and it can be recycled at this time. At present, most titanium dioxide factories usually use steam heating to evaporate the water in the waste titanium dioxide acid in the reactor or evaporator. Although the efficiency of concentrating the waste titanium dioxide acid in this way is relatively high, the actual production During the process, accidents such as high-temperature fouling and concentrated slurry blockage of heat exchangers or pipelines will occur, which will seriously affect the operating rate of the plant. Moreover, since the concentration of waste acid is carried out at high temperatures, the requirements for equipment are very high, and the investment is large. and higher maintenance costs.
发明内容Contents of the invention
本发明的目的是为了克服上述背景技术的不足，提供一种利用硫酸生产尾气提浓钛白废酸的方法，具有设备简单、操作方便、投资较少、能耗低、运行和维修费用较低、能够避免高温结垢、换热器或管道被堵塞的优点，并且还能给硫酸生产尾气的治理减轻压力。The purpose of the present invention is to overcome the deficiency of the above-mentioned background technology and provide a method for using sulfuric acid to produce tail gas to concentrate titanium dioxide waste acid, which has the advantages of simple equipment, convenient operation, less investment, low energy consumption, and low operation and maintenance costs , It can avoid the advantages of high temperature fouling, blockage of heat exchangers or pipelines, and it can also reduce the pressure for the treatment of sulfuric acid production tail gas.
本发明提供的利用硫酸生产尾气提浓钛白废酸的方法，包括下述步骤：(1)向喷淋成雾状的钛白废酸中通入硫酸生产尾气，对钛白废酸进行提浓，硫酸生产尾气由干燥气体变成含水蒸气和钛白废酸沫的湿气体；(2)将湿气体进行气液分离，将分离出来的气体进行处理后排空，分离出来的液体与经步骤(1)提浓过的钛白废酸混合后重复进行提浓操作；(3)对经多次提浓后的钛白废酸进行取样检测，待检测到钛白废酸中的硫酸含量按质量百分比计达到55％以上时即可回收钛白废酸。The method for using sulfuric acid to produce tail gas to concentrate titanium white waste acid provided by the invention comprises the following steps: (1) passing sulfuric acid into the titanium white waste acid sprayed into mist to produce tail gas, and extracting titanium white waste acid concentrated, sulfuric acid production tail gas is changed from dry gas to wet gas containing water vapor and titanium white waste acid foam; (2) the wet gas is separated into gas and liquid, and the separated gas is emptied after treatment, and the separated liquid is separated from the Step (1) Repeat the concentration operation after mixing the concentrated titanium dioxide waste acid; (3) Sampling and testing the titanium dioxide waste acid after multiple concentration, the sulfuric acid content in the titanium dioxide waste acid is to be detected Titanium white waste acid can be recovered when the mass percentage reaches more than 55%.
所述步骤(1)中喷淋成雾状的钛白废酸系通过若干螺旋喷头均匀喷淋而成。In the step (1), the titanium dioxide waste acid sprayed into mist is uniformly sprayed by several spiral spray nozzles.
硫酸生产尾气为从硫酸转化器出来的气体经吸收塔吸收后排出的废气，主要为含有少量二氧化硫、三氧化硫的氮气和氧气，由于是经吸收塔中的浓硫酸吸收过，因此该尾气为干燥气体。干燥的尾气与硫酸含量20％左右的钛白废酸充分接触，变为含饱和水蒸气和钛白废酸沫的湿气体，由于带走了钛白废酸中的水份，从而达到浓缩钛白废酸的目的。Sulfuric acid production tail gas is the waste gas discharged from the sulfuric acid converter after being absorbed by the absorption tower. It is mainly nitrogen and oxygen containing a small amount of sulfur dioxide and sulfur trioxide. Since it has been absorbed by the concentrated sulfuric acid in the absorption tower, the tail gas is dry gas. The dry tail gas is fully contacted with the waste titanium white acid with a sulfuric acid content of about 20%, and becomes a wet gas containing saturated water vapor and waste titanium white acid foam. Since the water in the waste titanium white acid is taken away, the concentration of titanium dioxide is achieved. The purpose of white waste acid.
与现有技术相比，本发明具有以下优点：Compared with the prior art, the present invention has the following advantages:
(1)设备简单，仅需要废酸槽、喷淋吸收塔、气液分离器和泵，废酸槽、喷淋吸收塔、气液分离器的材质均为聚氯乙烯PVC，投资非常少，运行和维修费用较低。(1) The equipment is simple, only waste acid tank, spray absorption tower, gas-liquid separator and pump are needed. The materials of waste acid tank, spray absorption tower and gas-liquid separator are all polyvinyl chloride PVC, and the investment is very small. Low operating and maintenance costs.
(2)能耗低，整个浓缩过程中无需高温加热或是减压蒸馏，除了废酸循环泵的电耗外，基本没有其它的能耗。(2) Low energy consumption, no high-temperature heating or vacuum distillation is required during the entire concentration process, and there is basically no other energy consumption except for the power consumption of the waste acid circulation pump.
(3)操作方便，由于浓缩装置与硫酸尾气治理装置连接在一起，系统比较稳定，运行过程没有温度压力等控制点，只需观察液位定时取样分析硫酸的含量，达到55％即浓缩完毕。(3) Easy to operate, because the concentrating device is connected with the sulfuric acid tail gas treatment device, the system is relatively stable, and there are no control points such as temperature and pressure during the operation process. It is only necessary to observe the liquid level and regularly take samples to analyze the content of sulfuric acid. When it reaches 55%, the concentration is complete.
(4)钛白废酸中的无机盐在高温下易生成硬质的垢，从而堵塞管道影响运行，本发明避开了高温，在常温下进行，主要设备采用耐稀酸腐蚀的PVC材料，克服了现有技术中设备腐蚀、高温结垢、结晶堵塞管道等缺陷。(4) Inorganic salts in titanium white waste acid are easy to generate hard scale at high temperature, thereby blocking the pipeline and affecting operation. The present invention avoids high temperature and is carried out at normal temperature. The main equipment adopts PVC material resistant to dilute acid corrosion. It overcomes the defects in the prior art such as equipment corrosion, high-temperature scaling, and crystallization to block pipelines.
(5)不仅对硫酸生产系统无任何影响，还能给硫酸生产尾气的处理减轻负担。本发明利用硫酸生产排放的干燥尾气带走水份来浓缩钛白废酸，不会对硫酸的产量、质量产生影响，即使浓缩装置出现故障停车，可以将喷淋吸收塔进气口、出气口关掉，让气体直接进入尾气处理装置。实际生产过程中，硫酸生产尾气经钛白废酸吸收后，气体中的三氧化硫浓度会变低，从而减轻尾气处理装置的负担。(5) Not only does it not have any impact on the sulfuric acid production system, but it can also reduce the burden on the treatment of sulfuric acid production tail gas. The invention utilizes the dry tail gas discharged from sulfuric acid production to take away water to concentrate titanium white waste acid, which will not affect the output and quality of sulfuric acid. Turn off and let the gas go directly to the exhaust treatment unit. In the actual production process, after sulfuric acid production tail gas is absorbed by titanium white waste acid, the concentration of sulfur trioxide in the gas will be reduced, thereby reducing the burden on the tail gas treatment device.
附图说明Description of drawings
图1为本发明暨实施例的工艺流程图。Fig. 1 is the process flow chart of the present invention and embodiment.
具体实施方式Detailed ways
下面结合附图及实施例对本发明作进一步的详细描述。The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
本发明实施例的浓缩设备比较简单，包括一个废酸槽、一个泵、一个喷淋吸收塔和一个气液分离器，其中，废酸槽、喷淋吸收塔和气液分离器均采用聚氯乙烯PVC材质制成。由于聚氯乙烯PVC色泽鲜艳、耐腐蚀、牢固耐用，并且在制造过程中增加了增塑剂、抗老化剂等一些辅助材料，因此，其耐热性、韧性、延展性比较好。废酸槽与喷淋吸收塔之间通过泵来循环物料，喷淋吸收塔内有若干个喷头，从位于喷淋吸收塔下部的进气口通入硫酸生产尾气，出气口连接气液分离器，进气口、出气口均通过蝶阀控制气量，气液分离器与硫酸尾气治理装置相连，经气液分离器分离的气体经硫酸尾气治理装置处理后排空，经气液分离器分离的液体回流进废酸槽。The concentration equipment of the embodiment of the present invention is relatively simple, including a waste acid tank, a pump, a spray absorption tower and a gas-liquid separator, wherein the waste acid tank, spray absorption tower and gas-liquid separator are all made of polyvinyl chloride Made of PVC material. Because polyvinyl chloride PVC has bright color, corrosion resistance, and durability, and some auxiliary materials such as plasticizers and anti-aging agents are added in the manufacturing process, its heat resistance, toughness, and ductility are relatively good. Pumps are used to circulate materials between the waste acid tank and the spray absorption tower. There are several nozzles in the spray absorption tower. The exhaust gas produced by sulfuric acid is introduced from the inlet located at the lower part of the spray absorption tower, and the gas outlet is connected to the gas-liquid separator. , the air inlet and outlet are controlled by butterfly valves, the gas-liquid separator is connected with the sulfuric acid tail gas treatment device, the gas separated by the gas-liquid separator is emptied after being treated by the sulfuric acid tail gas treatment device, and the liquid separated by the gas-liquid separator Return to waste acid tank.
在上述浓缩设备的基础上，本发明实施例提供的利用硫酸生产尾气提浓钛白废酸的方法工艺流程如下，参见图1所示：On the basis of the above-mentioned concentration equipment, the process flow of the method for using sulfuric acid to produce tail gas to concentrate titanium dioxide waste acid provided by the embodiment of the present invention is as follows, as shown in Figure 1:
将1250公斤钛白废酸投入废酸槽内，测得其硫酸含量为23.84％，开启泵，将废酸槽内的钛白废酸输送至喷淋吸收塔内，通过喷淋吸收塔上部安装的若干螺旋喷头均匀喷淋成雾状。开启喷淋吸收塔下部进气口控制气量的蝶阀，通入硫酸生产尾气，使上升的干燥尾气与喷淋吸收塔内向下喷淋的雾状钛白废酸相接触，对钛白废酸进行提浓，干燥尾气变成含饱和水蒸气和钛白废酸沫的湿气体。将湿气体通入气液分离器进行气液分离，将分离出来的气体通入硫酸尾气治理装置进行处理后排空，分离出来的液体回流进废酸槽，提浓过的钛白废酸亦进入废酸槽，混合后的钛白废酸重复进行提浓操作，连续运行53.17小时后，对经多次提浓后的钛白废酸进行取样检测，硫酸含量从23.84％提高到46.36％，滤去析出的无机盐等固态物料后，硫酸含量为58.45％，已经超过55％，可回收钛白废酸。Put 1250 kg of titanium dioxide waste acid into the waste acid tank, and the sulfuric acid content was measured to be 23.84%. Turn on the pump to transport the titanium dioxide waste acid in the waste acid tank to the spray absorption tower, and install it through the upper part of the spray absorption tower. A number of spiral nozzles spray evenly into mist. Open the butterfly valve at the air inlet at the lower part of the spray absorption tower to control the gas volume, and feed the tail gas produced by sulfuric acid to make the rising dry tail gas contact with the sprayed titanium dioxide waste acid sprayed downward in the spray absorption tower, and the titanium dioxide waste acid is treated. Concentrated, the dry tail gas becomes wet gas containing saturated water vapor and titanium white waste acid foam. The wet gas is passed into the gas-liquid separator for gas-liquid separation, and the separated gas is passed into the sulfuric acid tail gas treatment device for treatment and then emptied. The separated liquid flows back into the waste acid tank, and the concentrated titanium dioxide waste acid is also After entering the waste acid tank, the mixed titanium dioxide waste acid was repeatedly concentrated. After 53.17 hours of continuous operation, the titanium dioxide waste acid after repeated concentration was sampled and tested, and the sulfuric acid content increased from 23.84% to 46.36%. After filtering off the precipitated inorganic salt and other solid materials, the content of sulfuric acid is 58.45%, which has exceeded 55%, and the waste titanium dioxide acid can be recovered.
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| CN105293574B (en) * | 2015-10-26 | 2017-09-26 | 襄阳龙蟒钛业有限公司 | A kind of method of spent acid amount in reduction titanium white production |
| CN106289883A (en) * | 2016-08-02 | 2017-01-04 | 华电电力科学研究院 | Based on the portable sulfur trioxide sampling apparatus and the method that control condensation method |
| CN106268179B (en) * | 2016-08-25 | 2018-09-07 | 长沙有色冶金设计研究院有限公司 | A kind of energy saving technique and system of synthetical recovery sulfuric acid purification spent acid |
| CN110354916A (en) * | 2019-08-12 | 2019-10-22 | 国电环境保护研究院有限公司 | A carbon-based catalyst regeneration system |
| CN110624494A (en) * | 2019-10-31 | 2019-12-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Gas-liquid reactor for increasing the concentration of titanium dioxide waste acid |
| CN110642230A (en) * | 2019-10-31 | 2020-01-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for improving concentration of titanium white waste acid |
| CN113387334B (en) * | 2021-06-16 | 2022-10-28 | 龙佰四川钛业有限公司 | Concentration and purification method of titanium dioxide waste acid by sulfuric acid process |
| CN115925021A (en) * | 2022-11-07 | 2023-04-07 | 南通三圣石墨设备科技股份有限公司 | A Venturi thin film evaporation device and working method |
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