CN103820645A - Antimony pentachloride waste liquid treatment system - Google Patents
Antimony pentachloride waste liquid treatment system Download PDFInfo
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- CN103820645A CN103820645A CN201410107157.4A CN201410107157A CN103820645A CN 103820645 A CN103820645 A CN 103820645A CN 201410107157 A CN201410107157 A CN 201410107157A CN 103820645 A CN103820645 A CN 103820645A
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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 ofly for antimony pentachloride waste liquid being disposed to reclaim the system of weisspiessglanz, belong to antimony pentachloride waste liquid disposal technology field.
Background technology
Complicated component in antimony pentachloride waste liquid, existing recovery process and equipment, often ignored wherein collection and the recovery of acidic component and chloroform, and atmospheric environment has around been caused to destruction, and surrounding enviroment staff health causes and endangered.
Chinese patent literature CN102220496A discloses a kind of method that reclaims antimony peroxide from waste antimony pentachloride serving as fluorination catalyst, and A, extraction extract waste antimony pentachloride serving as fluorination catalyst with extraction agent, obtain 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 is directly under agitation added to water or antimony oxidation solution is mixed with aluminium salt after under agitation add again these two kinds of modes of water that antimony oxidation solution is hydrolyzed, filter and wash with water and obtain antimony peroxide.
Aforesaid method is not thorough to the processing of antimony pentachloride waste liquid, cuts and is unfavorable for collecting sour gas and the chloroform that reaction produces.
Summary of the invention
The present invention is directed to the deficiency that existing antimony pentachloride waste liquid recycling disposal technology exists, providing 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 collected sour gas and chloroform that reaction produces, 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, one-level film-falling 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 is joined with a point flow container, and the venting port of point flow container is connected with one-level film-falling absorption tower, and the leakage fluid dram of point flow container is connected with diluted acid storage tank and chloroform storage tank respectively; One-level film-falling absorption tower bottom connects the 4th in-line pump, the 4th in-line pump connects the top of one-level film-falling absorption tower, the venting port on one-level film-falling absorption tower top is connected with secondary film-falling absorption tower, the bottom of secondary film-falling absorption tower connects the 3rd in-line pump, the 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 and secondary film-falling absorption tower are all connected with vacuum buffer tank, 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) hydrolysis: pass into antimony pentachloride waste liquid by sewer pipe in primary first-order equation still, 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, in reaction, send large calorimetric, by pass into circulating water in primary first-order equation still, control temperature of reaction is 70-85 ℃; Reaction process is emitted tail gas (hydrogen chloride gas and chloroform gas), and tail gas enters graphite condenser, one-level film-falling 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 micro-negative pressure-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 too high in fruit acid concentration, pH value is less than at 3 o'clock, adds 32% liquid caustic soda to regulate reaction solution acidity by alkali liquid tank, so that metaantimmonic acid is separated out is more complete;
(3) by vacuum filtration machine, the reaction solution in primary first-order equation still is carried out to suction filtration, to the solid calcination processing producing; Filtrate is sent into and in secondary reaction still, is carried out secondary neutralization;
(4) in secondary and direct employing unslaked lime adds unslaked lime powder in secondary reaction still, and it is 60-80 ℃ that secondary reaction still makes temperature in it by steam heating, reacts 1 hour, and steam off after completion of the reaction, is down to room temperature by circulating water;
(5) mixing solutions producing after reaction in secondary reaction still is sent into pressure filter press filtration, and filtrate enters secondary filtrate tank, is pumped into Sewage treatment systems processes by second pipe;
(6) graphite condenser condensation is got off diluted acid and chloroform mixed solution enter a point flow container, enter respectively diluted acid storage tank and chloroform storage tank after natural layering, utilize.
The present invention has not only well reclaimed the weisspiessglanz in waste liquid, but also has collected sour gas and chloroform that reaction produces, and whole removal process can not impact environment, and the hydrogen cloride concentration steaming 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, one-level film-falling 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, one-level film-falling 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, it is interior with agitator and chuck, and be furnished with refrigeration cycle water lines and steam-heated cal(l)andria pipeline, the import of refrigeration cycle water lines is connected with the total return pipe 18 of water coolant and the total inlet pipe 19 of water coolant respectively with outlet, and steam-heated cal(l)andria pipeline is all connected with steam house steward 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, the first in-line pumps 24 and is connected with secondary reaction still 2.Primary first-order equation still 1 is also connected with alkali liquid tank 16, and neutralization reaction provides alkali lye for one time.On secondary reaction still 2, be 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.In graphite condenser 5, be provided with chuck and be furnished with refrigeration cycle water lines, and be connected with the total return pipe 18 of water coolant and the total inlet pipe 19 of water coolant, the outlet of graphite condenser 5 is joined with a point flow container 6, divide the venting port of flow container 6 to be connected with one-level film-falling 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.One-level film-falling absorption tower 3 bottoms connect the 4th in-line pump 27, the 4th in-line pump 27 connects the top of one-level film-falling absorption tower 3, the venting port on one-level film-falling absorption tower 3 tops 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, the 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.The vacuum port of secondary reaction still 2, first-level filtering flow container 11 and secondary film-falling absorption tower 4 is all connected with vacuum buffer tank 13, 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, and the aqueous solution in vacuum water tank, for alkalescence, is thoroughly absorbed the remaining sour gas in tail gas.
The operational process of said system comprises the following steps:
(1) hydrolysis
Pass into antimony pentachloride or butter of antimony waste liquid by sewer pipe 21 to primary first-order equation still 1.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.In reaction, send large calorimetric, by pass into circulating water in neutralizing hydrolysis reactor 1 chuck, keep the temperature of mixed solution in neutralizing hydrolysis the first reactor at 70 ℃-85 ℃.If waste liquid feed rate slows down, observe anhydrous acid tensimeter pressure, when insufficient pressure 0.2MPa, open anhydrous acid nitrogen pressure system, guarantee the reinforced smoothly of waste liquid.
(2) open vacuum pump 14, regulate vacuum pressure to be-0.01MPa.In vacuum pump 14, add the liquid caustic soda of mass concentration 15%, 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 is emitted hydrogen chloride gas, and tail gas (being hydrogen chloride gas and chloroform gas) enters graphite condenser 5, one-level film-falling absorption tower 3, secondary film-falling absorption tower 4 and alkali lye vacuum pump 14 successively.Micro-negative pressure-the 0.01MPa of the interior maintenance of neutralizing hydrolysis reactor 1, not obvious to guarantee the malleation in neutralizing hydrolysis reactor 1.
High for guaranteeing the hydrogen cloride concentration steaming, temperature of reaction is controlled at 80 ℃ of left and right, 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, be down to room temperature.Measure the acidity of neutralizing hydrolysis the first reactor 1 interior reaction solution, 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 to regulate reaction solution acidity by alkali liquid tank 16 at this, so that metaantimmonic acid is separated out is more complete, and reduces vacuum filtration machine 9 and operate 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 producing is the mixture of metaantimmonic acid and antimonous oxide, can send to incinerator and burn, the antimonous oxide obtaining and the mixture of antimony peroxide can be used as fire retardant and sell outward.Filtrate is the fluoride waste of hydrochloric acid and hydrofluoric acid and sodium-chlor, Sodium Fluoride, merges, and sends into and in secondary reaction still 2, carries out secondary neutralization.
(5) in secondary and direct employing unslaked lime, low price.Can adopt airtight solid material feeder directly to add unslaked lime powder by the opening for feed of secondary reaction still 2, unslaked lime consumption is theoretical consumption 110%.Secondary reaction still 2 makes temperature 60-80 ℃ in it by steam heating, reacts 1 hour, and steam off after completion of the reaction, opens cooling circulating water, is down to room temperature.While adding medicament, open the vacuum valve of reactor, make reactor produce micro-vacuum state, can avoid irritating smell to overflow, guarantee that again unslaked lime powder does not leak.
(6) the Calcium Fluoride (Fluorspan) mixing solutions that the interior reaction of secondary reaction still 2 produces is afterwards sent into pressure filter 10 press filtrations, 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) graphite condenser 5 condensations are got off diluted acid and chloroform mixed solution enter point flow container 6, enter respectively diluted acid storage tank 7 and chloroform storage tank 8 after natural layering, fully utilize.
Claims (1)
1. an antimony pentachloride waste liquid disposal system, comprises primary first-order equation still, secondary reaction still, one-level film-falling 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 is joined with a point flow container, and the venting port of point flow container is connected with one-level film-falling absorption tower, and the leakage fluid dram of point flow container is connected with diluted acid storage tank and chloroform storage tank respectively; One-level film-falling absorption tower bottom connects the 4th in-line pump, the 4th in-line pump connects the top of one-level film-falling absorption tower, the venting port on one-level film-falling absorption tower top is connected with secondary film-falling absorption tower, the bottom of secondary film-falling absorption tower connects the 3rd in-line pump, the 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 and secondary film-falling absorption tower are all connected with vacuum buffer tank, 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) hydrolysis: pass into antimony pentachloride waste liquid by sewer pipe in primary first-order equation still, 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, in reaction, send large calorimetric, by pass into circulating water in primary first-order equation still, control temperature of reaction is 70-85 ℃; Reaction process is emitted tail gas (hydrogen chloride gas and chloroform gas), and tail gas enters graphite condenser, one-level film-falling 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 micro-negative pressure-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 too high in fruit acid concentration, pH value is less than at 3 o'clock, adds 32% liquid caustic soda to regulate reaction solution acidity by alkali liquid tank, so that metaantimmonic acid is separated out is more complete;
(3) by vacuum filtration machine, the reaction solution in primary first-order equation still is carried out to suction filtration, to the solid calcination processing producing; Filtrate is sent into and in secondary reaction still, is carried out secondary neutralization;
(4) in secondary and direct employing unslaked lime adds unslaked lime powder in secondary reaction still, and it is 60-80 ℃ that secondary reaction still makes temperature in it by steam heating, reacts 1 hour, and steam off after completion of the reaction, is down to room temperature by circulating water;
(5) mixing solutions producing after reaction in secondary reaction still is sent into pressure filter press filtration, and filtrate enters secondary filtrate tank, is pumped into Sewage treatment systems processes by second pipe;
(6) graphite condenser condensation is got off diluted acid and chloroform mixed solution enter a point flow container, enter respectively diluted acid storage tank and chloroform storage tank after natural layering, utilize.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110500587A (en) * | 2019-08-21 | 2019-11-26 | 东华工程科技股份有限公司 | A kind of danger liquid waste incineration pretreatment system and processing 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 |
| CN114713294A (en) * | 2021-01-06 | 2022-07-08 | 中昊晨光化工研究院有限公司 | Treatment system and treatment method of waste antimony pentachloride catalyst |
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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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US6800786B1 (en) * | 2002-09-25 | 2004-10-05 | Baxter International, Inc. | Preparation of desflurane |
| 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110500587A (en) * | 2019-08-21 | 2019-11-26 | 东华工程科技股份有限公司 | A kind of danger liquid waste incineration pretreatment system and processing method |
| 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 |
| CN114713294A (en) * | 2021-01-06 | 2022-07-08 | 中昊晨光化工研究院有限公司 | Treatment system and treatment method of waste antimony pentachloride catalyst |
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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. |