CN104857827B - A kind of oleum neutralisation treatment device and technique for sulfonation production - Google Patents

A kind of oleum neutralisation treatment device and technique for sulfonation production Download PDF

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CN104857827B
CN104857827B CN201510108534.0A CN201510108534A CN104857827B CN 104857827 B CN104857827 B CN 104857827B CN 201510108534 A CN201510108534 A CN 201510108534A CN 104857827 B CN104857827 B CN 104857827B
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oleum
gas
liquid
wash tower
neutralizing tank
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CN104857827A (en
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赵昶
肖剑
万爱华
周西勇
肖凤军
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Guangzhou Liby Enterprise Group Co Ltd
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Guangzhou Liby Enterprise Group Co Ltd
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Abstract

The invention discloses a kind of oleum neutralisation treatment device and technique for sulfonation production.The neutralisation treatment device includes:Oleum neutralizing tank, gas-liquid separator, electrostatic precipitator, caustic wash tower, alkali cleaning circulating pump, liquid caustic soda storage tank, liquid caustic soda pump.The oleum neutralizing tank and caustic wash tower UNICOM;The oleum neutralizing tank top connects gas-liquid separator, the gas-liquid separator outlet connection electrostatic precipitator, the electrostatic precipitator outlet connection caustic wash tower;The liquid caustic soda storage tank is used for storing liquid caustic soda, and the liquid caustic soda is added in caustic wash tower by liquid caustic soda pump.Neutralisation treatment of the present invention for oleum in SO 3 sulfonated production process, avoid oleum and be passed directly in caustic wash tower and cause that tail gas acid mist amount is big, it is more to bubble, the exceeded phenomenon of tail gas harmful gass, effectively increases vent gas treatment effect when oleum is discharged.

Description

A kind of oleum neutralisation treatment device and technique for sulfonation production
Technical field
The present invention relates to a kind of oleum neutralisation treatment technique, is belonged to daily use chemicals industry and is given birth to by SO 3 sulfonated technique The technical field of sulfonated product is produced, the neutralisation treatment dress of oleum in more particularly to a kind of SO 3 sulfonated production process Put and technique.
Background technology
The surfactant base that daily use chemicals industry Betengent product is commonly used, such as LAS, AES, AS, AOS, MES etc. are generally Produced by SO 3 sulfonated technique, oleum, smoke can be produced in SO 3 sulfonated production process Sulphuric acid can all be produced to equipment and product quality and be had a strong impact on, accordingly, it would be desirable to collect oleum in process of production laggard Row is focused on.
Oleum compressed air after the oleum of prior art is processed typically by collection is pressed directly into alkali cleaning Absorbed in tower, this processing method is short because of flow process, oleum is short for time of contact with alkali liquor so that more oleum can not Absorbed in time and escaped washing tower (for removing CO2), a large amount of white acid mists are formed in offgas outlet, and with serious penetrating odor, so as to affect Arrive workshop surrounding.
Content of the invention
For the shortcoming and defect that oleum processing procedure is present, it is an object of the invention to provide a kind of be used for sulfonation The oleum neutralisation treatment device of production, it is to avoid oleum is passed directly in caustic wash tower and causes that tail gas acid mist amount is big, rises Many, the exceeded phenomenon of tail gas harmful gass is steeped, vent gas treatment effect when oleum is discharged is effectively increased.
Another object of the present invention is to providing in the oleum that a kind of use said apparatus carry out sulfonation production and place Science and engineering skill, it is big to solve oleum processing procedure tail gas acid mist amount, the penetrating odor technical problem such as again, is lifted at oleum Reason effect.
For reaching above-mentioned purpose, adopt the following technical scheme that:
A kind of oleum neutralisation treatment device for sulfonation production, which includes:Oleum neutralizing tank, gas-liquid separation Device, electrostatic precipitator, caustic wash tower, alkali cleaning circulating pump, liquid caustic soda storage tank, liquid caustic soda pump;The oleum neutralizing tank is joined with caustic wash tower Logical, the alkali liquor for neutralizing is circulated by alkali cleaning circulating pump;The oleum neutralizing tank top connects gas-liquid separator, The gas-liquid separator outlet connection electrostatic precipitator, the electrostatic precipitator outlet connection caustic wash tower;The liquid caustic soda storage tank is used In storage liquid caustic soda, the liquid caustic soda is added in caustic wash tower by liquid caustic soda pump.
The present invention oleum neutralisation treatment device, the oleum neutralizing tank be a hermetic container, oleum It is passed through.
The oleum neutralisation treatment device of the present invention, the acid mist of the oleum and generation that fail timely neutralization enter gas Liquid knockout drum, the liquid for separating are back to oleum neutralizing tank, and the gas for separating enters electrostatic precipitator.
The oleum neutralisation treatment device of the present invention, the gas after electrostatic precipitator enter caustic wash tower, use alkali liquor Sour gas is absorbed further, is then emptied.
The present invention oleum neutralisation treatment device, also include for detect control caustic wash tower in alkali liquor pH value Line pH meter, and carried out by automatic linkage scheme and liquid caustic soda pump chain.
In addition, the present invention also provides the oleum neutralisation treatment technique that a kind of use said apparatus carry out sulfonation production, Which comprises the following steps:
1), when production process needs to discharge oleum, oleum is pressed into oleum neutralizing tank, in oleum It is neutralized with circulation alkali liquor in neutralizing tank;
2) acid mist of the oleum acid mist and generation that fail timely neutralization enters gas-liquid separator;
3) gas after above-mentioned gas-liquid separator separates enters electrostatic precipitator, further removes acid mist;
4) tail gas and then after removing acid mist enters back into caustic wash tower, is further absorbed with alkali liquor and empty after sour gas.
The oleum neutralisation treatment technique of the present invention, step 1) in, the oleum compressed air of collection is pressed onto to be sent out In cigarette sulphuric acid neutralizing tank, reaction is neutralized with the alkali liquor in oleum neutralizing tank, with most of oleum in alkali liquor.
The present invention oleum neutralisation treatment technique, step 1) described in alkali liquor by online pH meter detection control ph Constant.Online pH meter is chain with liquid caustic soda pump.
The oleum neutralisation treatment technique of the present invention, step 2) in, it is back to by the liquid that gas-liquid separator is separated Oleum neutralizing tank.
As a result of above technical scheme, the invention has the advantages that and beneficial effect:
1), in oleum neutralisation treatment device of the invention, oleum neutralizing tank causes oleum neutralization reaction to exist Carry out in one hermetic container, the acid mist and tail gas of effusion will not be directly entered air;Knockout drum further removes tail gas In liquid component, so as to reduce electrostatic precipitator load;Electrostatic precipitator then can effectively remove the acid mist in tail gas;Most Afterwards when caustic wash tower, alkali liquor can absorb the sour gas such as sulfur dioxide therein and a small amount of sulfur trioxide, reach thoroughly clear The purpose that removes.
2) time that of the invention oleum neutralisation treatment prolonged process oleum is present in systems so as to Absorb to more fully neutralization, considerably reduce the amount that sulfuric acid mist escapes caustic wash tower;In whole oleum processing procedure, Caustic wash tower circulating pump causes alkali liquor in oleum neutralizing tank to be circulated, it is ensured that alkali liquor pH stable.
Description of the drawings
Fig. 1 is structural representation of the present invention for the oleum neutralisation treatment device of sulfonation production.
10:Oleum neutralizing tank 20:Gas-liquid separator
30:Electrostatic precipitator 40:Caustic wash tower
50:Alkali cleaning circulating pump 60:Liquid caustic soda storage tank
70:Liquid caustic soda pump 80:Online pH meter
Specific embodiment
Below in conjunction with the accompanying drawings with concrete preferred embodiment, the present invention is described in further detail.
As shown in figure 1, the present invention is for oleum neutralisation treatment device during sulfonation production, its structure is mainly wrapped Include:Oleum neutralizing tank 10, gas-liquid separator 20, electrostatic precipitator 30, caustic wash tower 40, alkali cleaning circulating pump 50, liquid caustic soda storage tank 60th, liquid caustic soda pump 70 and online pH meter 80.The top connection gas-liquid separator 20 of the oleum neutralizing tank 10.The gas-liquid separator 20 outlet connection electrostatic precipitator 30.The outlet connection caustic wash tower 40 of the electrostatic precipitator 30.The oleum neutralizing tank 10 With 40 UNICOM of caustic wash tower, the alkali liquor for neutralizing is circulated by alkali cleaning circulating pump 50, and the pH value of alkali liquor is by online pH meter 80 are tested and analyzed, and online pH meter and liquid caustic soda pump 70 carry out automatic interlock, the connection liquid caustic soda of liquid caustic soda pump 70 storage tank 80, for by liquid Alkali is squeezed into caustic wash tower 40 to keep stablizing for pH value.
The oleum neutralizing tank 10 is a hermetic container, the internal alkali liquor for filling about 1/3 height, oleum inlet tube Enter from oleum neutralizing tank top, the mouth of pipe submerges below liquid level, 316L material of the oleum inlet pipeline using DN25 Seamless steel pipe, upper gas outlet size be DN250.Oleum is passed through, and fails neutralization in time Oleum and the acid mist of generation enter gas-liquid separator 20, the liquid for separating is back to oleum neutralizing tank 10.
The gas-liquid separator 20 is a hermetic container, makes flow slowing down using its internal diameter for amplifying suddenly, so that bringing about the desired sensation The droplet carried in body is detained, and reaches the effect for separating gas-liquid.The gas that gas-liquid separator 20 is separated enters electrostatic demisting Device 30, the gas after electrostatic demisting 30 enter caustic wash tower 40, further absorb sour gas with alkali liquor, then empty.
The neutralisation treatment device of the present invention is the tail gas treating unit equipment using former sulfonation system, collectively constitutes one and sends out The neutralisation treatment device of cigarette sulphuric acid carries out the neutralisation treatment technique of oleum in SO 3 sulfonated production process.
Neutralisation treatment technique of the above-mentioned neutralisation treatment device to oleum in SO 3 sulfonated production process, can table State as follows:
Before discharge oleum, first open liquid caustic soda pump 70 and a certain amount of liquid caustic soda is squeezed into in caustic wash tower 40, by online The detection pH value of pH meter 80 reaches 10, then opens liquid caustic soda circulating pump (alkali cleaning circulating pump 50) to oleum neutralizing tank 10 Valve, is circulated the alkali liquor in oleum neutralizing tank 10, and it is stable to adjust alkali liquor pH.Then oleum is compressed Air press-in oleum neutralizing tank 10 is neutralized reaction with the alkali liquor of circulation, the oleum for failing neutralization in time and escaping Gas enters gas-liquid separator 20, and after gas-liquid separator 20 removes wherein acid mist and drop, gas enters electrostatic precipitator 30.Electrostatic precipitator 30 can further remove oleum acid mist therein, and then gas enters caustic wash tower 40, in caustic wash tower 40 Alkali liquor re-absorption sulfur dioxide therein and sulfur trioxide.This technical process efficiently can remove in oleum and when release big Amount acid mist and the gas with penetrating odor, tail gas when discharging oleum reach the normal level of production.
With reference to the process of the case study on implementation specific explanations present invention, but the enforcement of the present invention is not limited to following shape Formula.
Embodiment 1
As shown in figure 1, the present invention is a kind of for cigarette acid neutralizing unit in sulfonation production, the device includes nicotinic acid neutralizing tank 10, gas-liquid separator 20, electrostatic precipitator 30, caustic wash tower 40, alkali cleaning circulating pump 50, online pH meter 80 etc..The nicotinic acid neutralizing tank Top is connected with gas-liquid separator 20, and gas-liquid separator 20 is connected with electrostatic precipitator 30, electrostatic precipitator 30 and caustic wash tower 40 Connection, constitutes gas treatment flow process.The caustic wash tower 40, caustic wash tower circulating pump 50 and online pH80 are followed in series to form alkali wash water and follow Ring control system.
The nicotinic acid neutralizing tank 10, alkali cleaning circulating pump 50 and caustic wash tower 40 are followed in series to form the cyclic system of nicotinic acid neutralizer System.The filler that middle part filling can make liquid well distributed in the caustic wash tower 40, such as Pall ring, Raschig ring etc., bottom filling alkalescence Liquid, such as dilute sodium hydroxide solution, at the half position of liquid height to caustic wash tower visor, 40 another access filling pipe of caustic wash tower Road and mend alkali pipeline, so as to maintain tower in liquid pH constant, pH value control more than 9.
Filling and identical alkali liquor in caustic wash tower 40 in the nicotinic acid neutralizing tank 10, charging quantity about neutralize the 1/3 of tank volume.
The electrostatic precipitator 30 is the honeycomb fashion high-pressure electrostatic demister supporting with xanthator ability.
When said apparatus are used for nicotinic acid neutralisation treatment in sulfonation production, comprise the following steps:
1) to 40 moisturizing of caustic wash tower to the water level for requiring, opening alkali cleaning circulating pump 50, and the size of circular flow is adjusted, with Tower inner stuffing can be defined by whole moistenings.
2) value of online pH meter 80 is set as 9, and making PH meter automatic control controls mend alkali system carries out benefit alkali to caustic wash tower 40, adjusts PH value.
3) electrostatic precipitator 30 is opened, adjusts the voltage and current of electrostatic precipitator 30 so as to normal operation.
4) the alkali liquor circulation line control valve of nicotinic acid neutralizing tank 10 after pH is stable, is opened, and alkali liquor is made in nicotinic acid neutralizing tank 10 Middle energy normal circulation flowing.
5) control valve of the nicotinic acid inlet pipeline of nicotinic acid neutralizing tank 10 is opened, nicotinic acid press-in neutralizing tank is neutralized suction Receive.Failing absorbed nicotinic acid mist in time and gas-liquid separator 20 being entered with air-flow, in gas-liquid separator 20, nicotinic acid mist is entered One step is separated, and is back to nicotinic acid neutralizing tank 10, is re-started neutralization and is absorbed.A small amount of acid mist can be because cannot separate completely Entirely and as air-flow enters electrostatic precipitator 30, electrostatic precipitator 30 can efficiently catch acid mist, so acid mist is removed through electrostatic Eliminated substantially after day with fog 30, but electrostatic precipitator pair then effectively can not be removed with the sulfur dioxide gas for drying.Residual The sulfur dioxide gas for staying and micro sulfur trioxide gas are then further absorbed after caustic wash tower 40 is entered to be removed.The present invention Neutralisation treatment device energy effectively solving nicotinic acid emission in fumes of sulphuric acid amount big, the problems such as penetrating odor is big.
In the present embodiment, the oleum neutralizing tank 10 in above-mentioned flow elements, gas-liquid separator 20 and and smoke The pipeline of sulfuric acid contact is using the PVC materials for being difficult to be corroded by oleum.
Embodiment 2
By taking the xanthator of certain sulfonation workshop 3.8t/h as an example, under exhaust treatment system normal operating condition, per 24 hours Carry out the neutralisation treatment operation of an oleum.
During process, adjustment caustic wash tower 40 in alkali liquor pH to more than 9, and open caustic wash tower circulating pump 50 to oleum neutralize The control valve of tank 10, makes the alkali liquor in oleum neutralizing tank 10 be circulated flowing in system, opens oleum and receives Valve between the oleum neutralizing tank of collector, using the compressed air that pressure is 0.2MPa, with 5m3The flow of/h is by sulfonation Nicotinic acid in nicotinic acid collecting pipe is blown in oleum neutralizing tank 10, closes compressed air after 10 minutes, closes nicotinic acid neutralizing tank 10 imported valve and the valve of alkali liquor circulation pipe, that is, complete a nicotinic acid neutralisation treatment operation.
Can be seen that from the correction data of table 1 below can effectively reduce nicotinic acid discharge using the neutralisation treatment technique of the present invention When sulfuric acid mist concentration, tail gas reaches level during normal production.
Nicotinic acid discharge detection data contrast before and after 1 neutralisation treatment PROCESS FOR TREATMENT of the present invention of table
During sulfonation production, the present invention avoids oleum for the neutralisation treatment technique of oleum and directly arranges When entering caustic wash tower, emptying tail gas acid mist amount is big, and the big phenomenon of penetrating odor effectively increases oleum treatment effect.
The above, is only presently preferred embodiments of the present invention, not makees any pro forma restriction to the present invention, therefore Every without departing from technical solution of the present invention content, any simply repaiied according to what the technical spirit of the present invention made to above example Change, equivalent variations and modification, still fall within the range of technical solution of the present invention.

Claims (7)

1. a kind of oleum neutralisation treatment device for sulfonation production, it is characterised in which includes:Oleum neutralizing tank, Gas-liquid separator, electrostatic precipitator, caustic wash tower, alkali cleaning circulating pump, liquid caustic soda storage tank, liquid caustic soda pump;The oleum neutralizing tank with Caustic wash tower UNICOM, the alkali liquor for neutralizing are circulated by alkali cleaning circulating pump;The oleum neutralizing tank top connects gas Liquid/gas separator, the gas-liquid separator outlet connection electrostatic precipitator, the electrostatic precipitator outlet connection caustic wash tower;The liquid Alkali storage tank is used for storing liquid caustic soda, and the liquid caustic soda is added in caustic wash tower by liquid caustic soda pump;
The acid mist of the oleum and generation that fail timely neutralization enters knockout drum, and the liquid for separating is back to oleum Neutralizing tank, the gas for separating enter electrostatic precipitator;Gas after electrostatic precipitator enters caustic wash tower, further with alkali liquor Sour gas is absorbed, is then emptied.
2. the oleum neutralisation treatment device for sulfonation production according to claim 1, it is characterised in that:Described Cigarette sulphuric acid neutralizing tank is a hermetic container, and oleum is passed through.
3. the oleum neutralisation treatment device for sulfonation production according to claim 1, it is characterised in that:Described Cigarette sulphuric acid neutralizing tank, knockout drum and the pipeline that contacts with oleum are using the PVC materials for being difficult to be corroded by oleum Matter.
4. the oleum neutralisation treatment device for sulfonation production according to claim 1, it is characterised in that:Also include For detecting the online pH meter of the pH value of alkali liquor in control caustic wash tower, and carried out by automatic linkage scheme and liquid caustic soda pump chain.
5. a kind of usage right requires that the device described in 1 carries out the oleum neutralisation treatment technique of sulfonation production, and its feature exists In comprising the following steps:
1) when production process needs to discharge oleum, oleum is pressed into oleum neutralizing tank, is neutralized in oleum It is neutralized with circulation alkali liquor in tank;
2) acid mist of the oleum acid mist and generation that fail timely neutralization enters gas-liquid separator;Separated by gas-liquid separator Liquid is back to oleum neutralizing tank;
3) gas after above-mentioned gas-liquid separator separates enters electrostatic precipitator, further removes acid mist;
4) tail gas and then after removing acid mist enters back into caustic wash tower, is further absorbed with alkali liquor and empty after sour gas.
6. oleum neutralisation treatment technique according to claim 5, it is characterised in that:Step 1) in, the smoke of collection Sulphuric acid compressed air is pressed onto in oleum neutralizing tank, is neutralized reaction, alkali liquor with the alkali liquor in oleum neutralizing tank The most of oleum of neutralization.
7. oleum neutralisation treatment technique according to claim 5, it is characterised in that:Step 1) described in alkali liquor pass through Online pH meter detects the constant of control ph, and online pH meter is chain with liquid caustic soda pump.
CN201510108534.0A 2015-03-12 2015-03-12 A kind of oleum neutralisation treatment device and technique for sulfonation production Active CN104857827B (en)

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CN109534534B (en) * 2018-11-14 2024-02-09 山东丽波日化股份有限公司 Method and device for treating sulfonated waste sulfuric acid in detergent production
CN113798062A (en) * 2021-10-09 2021-12-17 上海奥威日化有限公司 Sulfonated tail gas treatment method
CN113908658B (en) * 2021-10-25 2024-03-12 轻工业杭州机电设计研究院有限公司 Safe and environment-friendly treatment method and treatment system for generating dioxane by sulfonation device

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CN101670225B (en) * 2009-10-19 2012-01-18 浙江赞宇科技股份有限公司 Sulfonated tail gas cycle-absorption method and cycle-absorption system
CN101966419A (en) * 2010-09-01 2011-02-09 浙江赞宇科技股份有限公司 Sulfur trioxide tail gas treating device in sulfonation reaction
CN102513039B (en) * 2011-12-26 2013-11-06 嘉兴赞宇科技有限公司 Sulfonated tail gas recycling method and sulfonated tail gas recycling system
CN202387445U (en) * 2011-12-26 2012-08-22 嘉兴赞宇科技有限公司 Recycling system for sulfonated tail gas
CN204563913U (en) * 2015-03-12 2015-08-19 广州立白企业集团有限公司 A kind of oleum neutralisation treatment device for sulfonation production

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