CN103820645B - Antimony pentachloride waste liquid treatment system - Google Patents
Antimony pentachloride waste liquid treatment system Download PDFInfo
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- CN103820645B CN103820645B CN201410107157.4A CN201410107157A CN103820645B CN 103820645 B CN103820645 B CN 103820645B CN 201410107157 A CN201410107157 A CN 201410107157A CN 103820645 B CN103820645 B CN 103820645B
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- Y—GENERAL 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
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Abstract
The invention provides an antimony pentachloride waste liquid treatment system. The antimony pentachloride waste liquid treatment system mainly comprises a primary reaction kettle and a secondary reaction kettle, wherein the primary reaction kettle is sequentially connected to a vacuum filtration machine, a first-stage filtrate tank, a first pipeline pump and the secondary reaction kettle; the secondary reaction kettle is sequentially connected to a filter press, a secondary-stage filtrate tank, a second pipeline pump and a wastewater treatment system; the primary reaction kettle is sequentially connected to a graphene condenser, a liquid distribution tank and a first-stage falling film absorption tower, and the liquid distribution tank is respectively connected to a dilute acid storage tank and a chloroform storage tank; the first-stage falling film absorption tower is sequentially connected to a fourth pipeline pump, the first-stage falling film absorption tower, a secondary-stage falling film absorption tower and a third pipeline pump; the secondary reaction kettle, the first-stage filtrate tank and the secondary-stage falling film absorption tower are connected to a vacuum buffer tank which is connected to a vacuum pump. The antimony pentachloride waste liquid treatment system can be used for recovering antimony oxide in waste liquid very well and collecting acid gas and chloroform generated in a reaction process and is complete in treatment and good in effect.
Description
Technical field
The present invention relates to a kind of system for disposing to reclaim weisspiessglanz to antimony pentachloride waste liquid, belong to antimony pentachloride waste liquid disposal technology field.
Background technology
Complicated component in antimony pentachloride waste liquid, existing recovery process and equipment, often have ignored collection and the recovery of wherein acidic component and chloroform, cause destruction to the atmospheric environment of surrounding, causes surrounding enviroment staff health and endanger.
Chinese patent literature CN102220496A discloses a kind of method reclaiming antimony peroxide from waste antimony pentachloride serving as fluorination catalyst, and A, extraction, extract waste antimony pentachloride serving as fluorination catalyst with extraction agent, obtains the inorganic phase extract containing antimony ion; B, oxidation, be oxidized inorganic phase extract with oxygenant, obtains antimony oxidation solution; C, hydrolysis, adopt antimony oxidation solution directly under agitation to be added water or under agitation add these two kinds of modes of water after being mixed with aluminium salt by antimony oxidation solution again antimony oxidation solution be hydrolyzed, and filters and wash with water to obtain antimony peroxide.
Aforesaid method is thorough to the process of antimony pentachloride waste liquid, cuts the sour gas and chloroform that are unfavorable for collecting reaction generation.
Summary of the invention
The present invention is directed to the deficiency that existing antimony pentachloride devil liquor recovery disposal technology exists, thering is provided a kind of disposes thoroughly, effective antimony pentachloride waste liquid disposal system, this system has not only well reclaimed the weisspiessglanz in waste liquid, but also have collected sour gas and the chloroform of reaction generation, whole removal process can not impact environment.
Antimony pentachloride waste liquid disposal system of the present invention, by the following technical solutions:
This system, comprises primary first-order equation still, secondary reaction still, stage falling-film absorption tower, secondary film-falling absorption tower, graphite condenser, point flow container, diluted acid storage tank, chloroform storage tank, vacuum filtration machine, pressure filter, first-level filtering flow container, secondary filtrate tank, vacuum buffer tank and vacuum pump; The opening for feed of primary first-order equation still is connected with sewer pipe, primary first-order equation still is also connected with an alkali liquid tank, the leakage fluid dram of primary first-order equation still is connected with vacuum filtration machine, the filtrate outlet of vacuum filtration machine connects first-level filtering flow container, the outlet of first-level filtering flow container connects the first in-line pump, and the first in-line pump is connected with secondary reaction still; The leakage fluid dram of secondary reaction still is connected with pressure filter, and pressure filter is connected with secondary filtrate tank, and secondary filtrate tank connects second pipe pump, and second pipe pump outlet is connected to Sewage treatment systems; The gas discharge outlet of primary first-order equation still is connected with graphite condenser, and the outlet of graphite condenser connects with a point flow container, and the venting port of point flow container is connected with stage falling-film absorption tower, and the leakage fluid dram of point flow container is connected with diluted acid storage tank and chloroform storage tank respectively; Bottom, stage falling-film absorption tower connects the 4th in-line pump, 4th in-line pump connects the top on stage falling-film absorption tower, the venting port on top, stage falling-film absorption tower is connected with secondary film-falling absorption tower, the bottom of secondary film-falling absorption tower connects the 3rd in-line pump, 3rd in-line pump connects secondary film-falling absorption tower, and the top of secondary film-falling absorption tower connects vacuum buffer tank; Secondary reaction still, first-level filtering flow container are all connected with vacuum buffer tank with secondary film-falling absorption tower, and vacuum buffer tank is connected with vacuum pump, and vacuum pump is connected with alkali liquor pipe;
The operational process of said system is:
(1) be hydrolyzed: in primary first-order equation still, pass into antimony pentachloride waste liquid by sewer pipe, antimony pentachloride waste liquid add speed be 0.1-0.15t/h(ton/hour), and add tap water, the volume ratio of tap water and antimony pentachloride waste liquid is 12:1, large calorimetric is sent in reaction, by passing into circulating water in primary first-order equation still, control temperature of reaction is 70-85 DEG C; Reaction process releases tail gas (hydrogen chloride gas and chloroform gas), and tail gas enters graphite condenser, stage falling-film absorption tower, secondary film-falling absorption tower and vacuum pump successively; Open vacuum pump, regulate vacuum pressure to be-0.01MPa, in vacuum pump, add the liquid caustic soda of mass concentration 15%, to absorb residual exhaust, in primary first-order equation still, keep tiny structure-0.01MPa; Reinforced complete, close recirculated water, until tail gas is not obvious, reach environmental emission standard;
(2) after hydrolysis completely, make primary first-order equation still be down to room temperature, sampling and measuring reaction solution acidity, as fruit acid concentration is too high, when pH value is less than 3, adds 32% liquid caustic soda by alkali liquid tank and regulate reaction solution acidity, more complete to make metaantimmonic acid separate out;
(3) by vacuum filtration machine, suction filtration is carried out to the reaction solution in primary first-order equation still, to the solid calcination processing produced; Filtrate is sent in secondary reaction still and is carried out Two-step neutralization;
(4) Two-step neutralization directly adopts unslaked lime, in secondary reaction still, add unslaked lime powder, and secondary reaction still makes temperature in it be 60-80 DEG C by steam heating, and react 1 hour, steam off after completion of the reaction, is down to room temperature by circulating water;
(5) mixing solutions produced after reaction in secondary reaction still sends into pressure filter press filtration, and filtrate enters secondary filtrate tank, is pumped into Sewage treatment systems processes by second pipe;
(6) diluted acid that gets off of graphite condenser condensation and chloroform mixed solution enter a point flow container, enter diluted acid storage tank and chloroform storage tank respectively, utilize after natural layering.
The present invention has not only well reclaimed the weisspiessglanz in waste liquid, but also have collected sour gas and the chloroform of reaction generation, and whole removal process can not impact environment, and the hydrogen cloride concentration steamed is high, disposes thoroughly, effective.
Accompanying drawing explanation
Fig. 1 is the structural representation of antimony pentachloride waste liquid disposal system of the present invention.
In figure: 1, primary first-order equation still, 2, secondary reaction still, 3, stage falling-film absorption tower, 4, secondary film-falling absorption tower, 5, graphite condenser, 6, point flow container, 7, diluted acid storage tank, 8, chloroform storage tank, 9, vacuum filtration machine, 10, pressure filter, 11, first-level filtering flow container, 12, secondary filtrate tank, 13, vacuum buffer tank, 14, vacuum pump; 15, Sewage treatment systems; 16, alkali liquid tank, 17, alkali liquor pipe, 18, the total return pipe of recirculated water; 19, the total inlet pipe of recirculated water; 20, steam manifold; 21, sewer pipe; 22, compressed air pipe; 23, running water pipe; 24, the first in-line pump; 25, second pipe pump; 26, the 3rd in-line pump; 27, the 4th in-line pump.
Embodiment
As shown in Figure 1, antimony pentachloride waste liquid disposal system of the present invention comprises primary first-order equation still 1, secondary reaction still 2, stage falling-film absorption tower 3, secondary film-falling absorption tower 4, graphite condenser 5, point flow container 6, diluted acid storage tank 7, chloroform storage tank 8, vacuum filtration machine 9, pressure filter 10, first-level filtering flow container 11, secondary filtrate tank 12, vacuum buffer tank 13 and vacuum pump 14.Primary first-order equation still 1 and secondary reaction still 2 adopt popular response still structure, with agitator and chuck in it, and be furnished with refrigeration cycle water lines and steam-heated cal(l)andria pipeline, the import of refrigeration cycle water lines and outlet respectively return pipe 18 total with water coolant and the total inlet pipe 19 of water coolant are connected, and steam-heated cal(l)andria pipeline is all connected with steam main 20.Primary first-order equation still 1 is provided with opening for feed, compressed air inlet, gas discharge outlet and leakage fluid dram, opening for feed is connected with sewer pipe 21, compressed air inlet is connected with compressed air pipe 22, leakage fluid dram is connected with vacuum filtration machine 9, the filtrate outlet of vacuum filtration machine 9 connects first-level filtering flow container 11, the outlet of first-level filtering flow container 11 connects the first in-line pump 24, first in-line pump 24 and is connected with secondary reaction still 2.Primary first-order equation still 1 is also connected with alkali liquid tank 16, and for one time, neutralization reaction provides alkali lye.Secondary reaction still 2 is provided with opening for feed, vacuum interface and leakage fluid dram.The leakage fluid dram of secondary reaction still 2 is connected with pressure filter 10, and pressure filter 10 is connected with secondary filtrate tank 12, and secondary filtrate tank 12 connects second pipe pump 25, and the outlet of second pipe pump 25 is connected to Sewage treatment systems 15.The gas discharge outlet of primary first-order equation still 1 is connected with graphite condenser 5.Be provided with chuck in graphite condenser 5 and be furnished with refrigeration cycle water lines, and be connected with the total return pipe of water coolant 18 and the total inlet pipe 19 of water coolant, the outlet of graphite condenser 5 connects with a point flow container 6, divide the venting port of flow container 6 to be connected with stage falling-film absorption tower 3, the discharge opeing of point flow container 6 is connected with diluted acid storage tank 7 and chloroform storage tank 8 respectively.Bottom, stage falling-film absorption tower 3 connects the 4th in-line pump 27,4th in-line pump 27 connects the top on stage falling-film absorption tower 3, the venting port on top, stage falling-film absorption tower 3 is connected with secondary film-falling absorption tower 4, the bottom of secondary film-falling absorption tower 4 connects the 3rd in-line pump 26,3rd in-line pump 26 connects secondary film-falling absorption tower 4, and the top of secondary film-falling absorption tower 4 connects vacuum buffer tank 13.Secondary reaction still 2, first-level filtering flow container 11 are all connected with vacuum buffer tank 13 with the vacuum port of secondary film-falling absorption tower 4, and vacuum buffer tank 13 is connected with vacuum pump 14.Because vacuum pump 14 adopts water-ring vacuum pump, so vacuum pump 14 is connected with running water pipe 23, supplement fresh water.Vacuum pump 14 is connected with alkali liquor pipe 17, makes the aqueous solution in vacuum water tank be alkalescence, thoroughly absorbs the remaining sour gas in tail gas.
The operational process of said system comprises the following steps:
(1) be hydrolyzed
Antimony pentachloride or butter of antimony waste liquid is passed into primary first-order equation still 1 by sewer pipe 21.Open baiting valve, waste liquid slowly put into neutralizing hydrolysis reactor 1, waste liquid add speed according to 0.1-0.15t/h(ton/hour).The object of hydrolysis is the toxicity in order to eliminate antimony pentachloride and butter of antimony, and whole process need add tap water, and the volume ratio of tap water and antimony pentachloride waste liquid is 12:1.Sending large calorimetric in reaction, by passing into circulating water in neutralizing hydrolysis reactor 1 chuck, keeping the temperature of mixed solution in neutralizing hydrolysis first reactor at 70 DEG C-85 DEG C.If waste liquid feed rate slows down, observe anhydrous acid gage pressure, during insufficient pressure 0.2MPa, open anhydrous acid nitrogen pressure system, ensure the reinforced smoothly of waste liquid.
(2) open vacuum pump 14, regulate vacuum pressure to be-0.01MPa.Add the liquid caustic soda of mass concentration 15% in vacuum pump 14, open the 3rd in-line pump 26 and the 4th in-line pump 27, open the circulating water line of graphite condenser 5.Hydrolysis reaction releases hydrogen chloride gas, and tail gas (being hydrogen chloride gas and chloroform gas) enters graphite condenser 5, stage falling-film absorption tower 3, secondary film-falling absorption tower 4 and alkali lye vacuum pump 14 successively.Tiny structure-0.01MPa is kept in neutralizing hydrolysis reactor 1, not obvious to guarantee the malleation in neutralizing hydrolysis reactor 1.
High for ensureing the hydrogen cloride concentration steamed, temperature of reaction controls at about 80 DEG C, and the reinforced later stage can suitably reduce recirculated water aperture.Reinforced complete, close recirculated water, continue decompression vacuum pumping until acid mist (hydrogen chloride gas and chloroform gas) is not obvious, reach environmental emission standard.
(3), after hydrolysis completely, room temperature is down to.Measure the acidity of reaction solution in neutralizing hydrolysis first reactor 1, as too high in fruit acid concentration (pH value is less than 3), because antimonous oxide and metaantimmonic acid are all dissolved in concentrated acid, therefore in reaction solution, antimony content may be too high, if pH value is less than 3, can suitably add 32% liquid caustic soda at this by alkali liquid tank 16 and regulate reaction solution acidity, more complete to make metaantimmonic acid separate out, and also minimizing vacuum filtration machine 9 operates severe degree.
(4) adopt lining mould airtight vacuum suction filtration machine 9 in and the reacted fluid of hydrolytic reaction pot 1 carry out suction filtration, the solid produced is the mixture of metaantimmonic acid and antimonous oxide, can send to incinerator to burn, the antimonous oxide obtained and the mixture of antimony peroxide can be used as outside fire retardant to be sold.Filtrate is the fluoride waste of hydrochloric acid and hydrofluoric acid and sodium-chlor, Sodium Fluoride, merges, sends in secondary reaction still 2 and carry out Two-step neutralization.
(5) Two-step neutralization directly adopts unslaked lime, low price.Airtight solid material feeder can be adopted directly to add unslaked lime powder by the opening for feed of secondary reaction still 2, and unslaked lime consumption is 110% of theoretical amount.Secondary reaction still 2 makes temperature 60-80 DEG C in it by steam heating, and react 1 hour, steam off after completion of the reaction, opens cooling circulating water, is down to room temperature.When adding medicament, open the vacuum valve of reactor, make reactor produce micro-vacuum state, irritating smell namely can be avoided to overflow, ensure that again unslaked lime powder does not leak.
(6) the Calcium Fluoride (Fluorspan) mixing solutions produced after reaction in secondary reaction still 2 sends into pressure filter 10 press filtration, and filtrate enters secondary filtrate tank 12, sends into Sewage treatment systems 15 process by second pipe pump 24, and purer Calcium Fluoride (Fluorspan) is sold as fluorite after drying.
(7) diluted acid that gets off of graphite condenser 5 condensation and chloroform mixed solution enter point flow container 6, enter diluted acid storage tank 7 and chloroform storage tank 8 respectively, fully utilize after natural layering.
Claims (1)
1. an antimony pentachloride waste liquid disposal system, comprises primary first-order equation still, secondary reaction still, stage falling-film absorption tower, secondary film-falling absorption tower, graphite condenser, point flow container, diluted acid storage tank, chloroform storage tank, vacuum filtration machine, pressure filter, first-level filtering flow container, secondary filtrate tank, vacuum buffer tank and vacuum pump; It is characterized in that:
The opening for feed of primary first-order equation still is connected with sewer pipe, primary first-order equation still is also connected with an alkali liquid tank, the leakage fluid dram of primary first-order equation still is connected with vacuum filtration machine, the filtrate outlet of vacuum filtration machine connects first-level filtering flow container, the outlet of first-level filtering flow container connects the first in-line pump, and the first in-line pump is connected with secondary reaction still; The leakage fluid dram of secondary reaction still is connected with pressure filter, and pressure filter is connected with secondary filtrate tank, and secondary filtrate tank connects second pipe pump, and second pipe pump outlet is connected to Sewage treatment systems; The gas discharge outlet of primary first-order equation still is connected with graphite condenser, and the outlet of graphite condenser connects with a point flow container, and the venting port of point flow container is connected with stage falling-film absorption tower, and the leakage fluid dram of point flow container is connected with diluted acid storage tank and chloroform storage tank respectively; Bottom, stage falling-film absorption tower connects the 4th in-line pump, 4th in-line pump connects the top on stage falling-film absorption tower, the venting port on top, stage falling-film absorption tower is connected with secondary film-falling absorption tower, the bottom of secondary film-falling absorption tower connects the 3rd in-line pump, 3rd in-line pump connects secondary film-falling absorption tower, and the top of secondary film-falling absorption tower connects vacuum buffer tank; Secondary reaction still, first-level filtering flow container are all connected with vacuum buffer tank with secondary film-falling absorption tower, and vacuum buffer tank is connected with vacuum pump, and vacuum pump is connected with alkali liquor pipe;
The operational process of said system is:
(1) be hydrolyzed: in primary first-order equation still, pass into antimony pentachloride waste liquid by sewer pipe, the speed that adds of antimony pentachloride waste liquid is 0.1-0.15t/h, and add tap water, the volume ratio of tap water and antimony pentachloride waste liquid is 12:1, large calorimetric is sent in reaction, by passing into circulating water in primary first-order equation still, control temperature of reaction is 70-85 DEG C; Reaction process releases tail gas hydrogen chloride gas and chloroform gas, and tail gas enters graphite condenser, stage falling-film absorption tower, secondary film-falling absorption tower and vacuum pump successively; Open vacuum pump, regulate vacuum pressure to be-0.01MPa, in vacuum pump, add the liquid caustic soda of mass concentration 15%, to absorb residual exhaust, in primary first-order equation still, keep tiny structure-0.01MPa; Reinforced complete, close recirculated water, until tail gas is not obvious, reach environmental emission standard;
(2) after hydrolysis completely, make primary first-order equation still be down to room temperature, sampling and measuring reaction solution acidity, as fruit acid concentration is too high, when pH value is less than 3, adds 32% liquid caustic soda by alkali liquid tank and regulate reaction solution acidity, more complete to make metaantimmonic acid separate out;
(3) by vacuum filtration machine, suction filtration is carried out to the reaction solution in primary first-order equation still, to the solid calcination processing produced; Filtrate is sent in secondary reaction still and is carried out Two-step neutralization;
(4) Two-step neutralization directly adopts unslaked lime, in secondary reaction still, add unslaked lime powder, and secondary reaction still makes temperature in it be 60-80 DEG C by steam heating, and react 1 hour, steam off after completion of the reaction, is down to room temperature by circulating water;
(5) mixing solutions produced after reaction in secondary reaction still sends into pressure filter press filtration, and filtrate enters secondary filtrate tank, is pumped into Sewage treatment systems processes by second pipe;
(6) diluted acid that gets off of graphite condenser condensation and chloroform mixed solution enter a point flow container, enter diluted acid storage tank and chloroform storage tank respectively, utilize after natural layering.
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| CN201410107157.4A CN103820645B (en) | 2014-03-21 | 2014-03-21 | Antimony pentachloride waste liquid treatment system |
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| CN110500587B (en) * | 2019-08-21 | 2021-06-15 | 东华工程科技股份有限公司 | Hazardous waste liquid incineration pretreatment system and treatment method |
| CN110902719A (en) * | 2019-10-11 | 2020-03-24 | 江苏梅兰化工有限公司 | Method for recovering antimony trioxide from difluorochloromethane reaction residual liquid |
| CN111638286A (en) * | 2020-06-11 | 2020-09-08 | 盐城工学院 | Device for pretreating smelly water sample and operation process thereof |
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| CN100383053C (en) * | 2004-08-11 | 2008-04-23 | 巨化集团公司 | Method for recovering and making antimony oxide from antimony pentachloride solution |
| CN203782205U (en) * | 2014-03-21 | 2014-08-20 | 山东腾跃化学危险废物研究处理有限公司 | Antimony pentachloride waste liquid treatment system |
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Effective date of registration: 20190705 Address after: 251414 No. 1000, Beichencun, Renfeng Town, Jiyang County, Jinan City, Shandong Province Patentee after: Ji'nan cloud water leaping Environmental Protection Technology Co., Ltd. Address before: 250100 No. 1 Hot Spring Road, Lingang Development Zone, Jinan City, Shandong Province Patentee before: SHANDONG TENGYUE CHEMICAL HAZARDOUS WASTE RESEARCH & TREATMENT CO., LTD. |