CN106823667A - Chloride methane waste product handling process in a kind of paraquat production - Google Patents

Chloride methane waste product handling process in a kind of paraquat production Download PDF

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Publication number
CN106823667A
CN106823667A CN201710005404.3A CN201710005404A CN106823667A CN 106823667 A CN106823667 A CN 106823667A CN 201710005404 A CN201710005404 A CN 201710005404A CN 106823667 A CN106823667 A CN 106823667A
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CN
China
Prior art keywords
paraquat
waste product
chloromethanes
handling process
methane waste
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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
Application number
CN201710005404.3A
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Chinese (zh)
Inventor
袁晓路
王佳
孔军军
陈后福
杨志红
王新国
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Anhui Guoxing Biochemistry Co Ltd
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Anhui Guoxing Biochemistry Co Ltd
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Priority to CN201710005404.3A priority Critical patent/CN106823667A/en
Publication of CN106823667A publication Critical patent/CN106823667A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1406Multiple stage absorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1487Removing organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1493Selection of liquid materials for use as absorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18Absorbing units; Liquid distributors therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2252/00Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/10Inorganic absorbents
    • B01D2252/103Water
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2252/00Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20Organic absorbents
    • B01D2252/202Alcohols or their derivatives
    • B01D2252/2021Methanol
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/20Halogens or halogen compounds
    • B01D2257/206Organic halogen compounds
    • B01D2257/2064Chlorine
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/70Organic compounds not provided for in groups B01D2257/00 - B01D2257/602

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention provides chloride methane waste product handling process in a kind of paraquat production, the chloride methane waste product that paraquat synthesis reactor is discharged is passed into condenser and is condensed, then enter the chloromethanes tourie equipped with gas distributor by surge tank, chimney is entered after being absorbed using three-level.Using process of the invention, the components such as methyl alcohol in paraquat production process in alkylated reaction waste gas, pyridine and chloromethanes can be effectively reclaimed, the component for being reclaimed can be applied mechanically directly, improve chloromethanes utilization rate, production cost is reduced, waste gas discharge is reduced, there is good application value.

Description

Chloride methane waste product handling process in a kind of paraquat production
Technical field
The present invention relates to paraquat exhaust-gas treatment field, and in particular to chloride methane waste product treatment in a kind of paraquat production Technique.
Background technology
Paraquat, chemical name is 1-1- dimethyl -4-4- bipyridine cation salt, is a kind of quick total weed control Agent, with action of contace poison and certain systemic action, can be absorbed rapidly by plant green tissues, make its withered.Paraquat is to non-green Colour cell is knitted and not acted on, and is combined with soil rapidly in soil and is passivated, to plant root and perennial subterranean stem and perennial root without Effect.In recent years, the paraquat market demand rose in great-jump-forward, and good market prospects have been shown at present.
The synthetic technology of paraquat mainly has metallic sodium method and a sodium cyanide method, wherein metallic sodium method be divided into again high-temperature sodium method and Low temperature sodium method;Sodium cyanide method is divided into water cyanogen method, alcohol cyanogen method and ammonia cyanogen method.Metallic sodium method has been prohibited due to dangerous high factor Only paraquat product is produced using the process route.Sodium cyanide method process characteristic is that picolyl metaplasia first is produced into N- picolines Salt, then polymerisation is carried out, chlorine oxidation production paraquat.The methyl of introducing plays positioning action, coupling reaction is only occurred In contraposition, it is difficult to produce 2,2 ' and 2,4- bipyridyl and Polypyridine, it is ensured that paraquat product quality and production safety.Water cyanogen Method is carried out as solvent, alkylated reaction and dimerization reaction using water all in water, but ionic catalysis of the Cymag in water is lived Property is poor, and the input amount of cryanide ion is very big, yield only 75%, and organic by-products, cyanide content are high in waste water, intractability Greatly.Alcohol cyanogen method dimerization reaction is carried out in water and METHANOL MEDIUM, and yield brings up to 85%, but cryanide ion input amount and water cyanogen method phase When, and alcohol cyanogen method will reclaim hydrogen cyanide, with very big danger.The alkylation of ammonia cyanogen method is using methyl alcohol as solvent, and dimerization is anti- Should be carried out in liquefied ammonia atmosphere, there is no on fire and explosion danger, process is simple, smooth operation, while it is desirable to carried out under high pressure, But ensure that all ammonia solutions can be recycled.But ammonia cyanogen method is in insulating process is alkylated by pressure discharge operations by reactor Waste gas discharged, in waste gas contain a large amount of chloromethanes, also containing a small amount of methyl alcohol and pyridine, chloromethanes utilization rate is relatively low, tail Gas is directly discharged to pollute environment in air.
The content of the invention
In view of the shortcomings of the prior art, the invention provides chloride methane waste product handling process in a kind of production of paraquat.
To realize object above, the present invention is achieved by the following technical programs:
A kind of chloride methane waste product handling process in paraquat production, step is as follows:By containing that paraquat synthesis reactor is discharged Chloromethanes waste gas is condensed in being passed into condenser, then enters the chloromethanes tourie equipped with gas distributor by surge tank, Chimney is entered after being absorbed using three-level.
Preferably, it is methyl alcohol that the chloromethanes tourie first order absorbs the absorbing liquid for using.
Preferably, the methanol usage is 20-50 times of exhaust mass, after treatment exhausted air quantity reaches the 10-30% of deadweight Substitute the solvent that methyl alcohol is alkylated workshop section as paraquat.
Preferably, the chloromethanes tourie second level absorbs the absorbing liquid for using for mass fraction is the methyl alcohol of 50wt% The aqueous solution.
Preferably, the methanol aqueous solution consumption is 5-10 times of exhaust mass, and methanol content reaches in the absorbing liquid The solvent that methyl alcohol is alkylated workshop section as paraquat is substituted when more than 80%.
Preferably, it is water that the chloromethanes tourie third level absorbs the absorbing liquid for using.
Preferably, the consumption of the water is 2-5 times of absorbing liquid quality in two grades of touries, and methyl alcohol contains in the absorbing liquid Enter in the tourie of the second level when amount reaches more than 5% and prepare absorbing liquid.
Beneficial effect of the present invention:The invention provides chloride methane waste product handling process in one kind production, paraquat production In chloride methane waste product condense within the condenser, while cooling to waste gas by the methyl alcohol in air-flow, pyridine condensation reclaim, Condensed waste gas enters chloromethanes absorption tower by surge tank, by reaching emission request after three-level absorption, from smoke stack emission Into air.Using process of the invention, the first in alkylated reaction waste gas in paraquat production process can be effectively reclaimed The components such as alcohol, pyridine and chloromethanes, the component for being reclaimed can be applied mechanically directly, improve chloromethanes utilization rate, reduce production cost, Waste gas discharge is reduced, there is good application value.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention, Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one Divide embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making The every other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Chloride methane waste product treatment process design in paraquat production:What is given off in paraquat synthesis reactor is useless containing chloromethanes Gas first condensation cooling within the condenser, the component condensation liquefaction such as methyl alcohol, pyridine, realizes gas-liquid separation in surge tank in waste gas, Lower floor's liquid continues to participate in alkylated reaction in returning to alkylation synthesis reactor by pipeline, and top tank air absorbs into chloromethanes Tank, the absorbing liquid that first order tourie is used is methyl alcohol, for absorbing chloromethanes and not a small amount of uncooled methyl alcohol and pyridine, the The absorbing liquid that two grades of touries are used is methanol aqueous solution, for absorbing a small amount of chloromethanes and air-flow band in first order absorption outlet The methyl alcohol for going out, the absorbing liquid that third level tourie is used is clear water, for absorbing micro chloromethanes and two grades of absorption outlet gas A small amount of methyl alcohol and steam that stream is taken out of.Methyl alcohol/the pyridine mixtures collected in surge tank can be applied mechanically directly, the first of first order absorption During direct set uses paraquat production after alcohol absorption saturation, two grades of methanol aqueous solutions of absorption are after methanol content reaches 80% During directly set uses paraquat production, it is used to prepare two grades of absorbing liquids when methanol content reaches more than 5% in three-level absorbing liquid.
Embodiment 1:
Paraquat production alkylation synthesis reactor is vented chloride methane waste product 50.5kg, after condensation in surge tank methyl alcohol and pyrrole The mixed liquor 8.2kg of pyridine, first order absorption tank quantity of methyl alcohol is 2000kg, and increase weight 38.6kg after absorption chloromethanes, and two grades of touries are The methanol aqueous solution of 400kg50%, increase weight 1.8kg after absorption chloromethanes, and three-level tourie is the clear water of 1000kg, absorbs chloromethane Increased weight 0.3kg after alkane, and active principle 48.9kg, the rate of recovery 96.83% are reclaimed altogether.
Embodiment 2:
Paraquat production alkylation synthesis reactor is vented chloride methane waste product 49.8kg, after condensation in surge tank methyl alcohol and pyrrole The mixed liquor 8.1kg of pyridine, first order absorption tank quantity of methyl alcohol is 2500kg, and increase weight 36.2kg after absorption chloromethanes, and two grades of touries are The methanol aqueous solution of 500kg50%, increase weight 2.4kg after absorption chloromethanes, and three-level tourie is the clear water of 1200kg, absorbs chloromethane Increased weight 0.5kg after alkane, and active principle 47.2kg, the rate of recovery 94.78% are reclaimed altogether.
Embodiment 3:
Paraquat production alkylation synthesis reactor is vented chloride methane waste product 51.3kg, after condensation in surge tank methyl alcohol and pyrrole The mixed liquor 8.3kg of pyridine, first order absorption tank quantity of methyl alcohol is 1100kg, and increase weight 32.5kg after absorption chloromethanes, and two grades of touries are The methanol aqueous solution of 300kg50%, increase weight 4.5kg after absorption chloromethanes, and three-level tourie is the clear water of 800kg, absorbs chloromethane Increased weight 0.6kg after alkane, and active principle 45.9kg, the rate of recovery 89.47% are reclaimed altogether.
Embodiment 4:
Paraquat production alkylation synthesis reactor is vented chloride methane waste product 49.7kg, after condensation in surge tank methyl alcohol and pyrrole The mixed liquor 7.8kg of pyridine, first order absorption tank quantity of methyl alcohol is 1000kg, and increase weight 27.6kg after absorption chloromethanes, and two grades of touries are The methanol aqueous solution of 250kg50%, increase weight 5.6kg after absorption chloromethanes, and three-level tourie is the clear water of 1200kg, absorbs chloromethane Increased weight 0.8kg after alkane, and active principle 41.8kg, the rate of recovery 84.10% are reclaimed altogether.
Embodiment 5:
Paraquat production alkylation synthesis reactor is vented chloride methane waste product 200kg, after condensation in surge tank methyl alcohol and pyrrole The mixed liquor 30kg of pyridine, first order absorption tank quantity of methyl alcohol is 7900kg, and increase weight 148kg after absorption chloromethanes, and two grades of touries are The methanol aqueous solution of 1500kg50%, increase weight 10kg after absorption chloromethanes, and three-level tourie is the clear water of 3800kg, absorbs chloromethane Increased weight 2.5kg after alkane, and active principle 190.5kg, the rate of recovery 95.25% are reclaimed altogether, wherein reclaiming methyl alcohol 36.8kg, pyridine 4.3kg, chloromethanes 149.4kg.Condensate liquid and first order absorption liquid are directly applied mechanically, paraquat yield is constant.
Embodiment 6:
Paraquat production alkylation synthesis reactor is vented chloride methane waste product 50kg, after condensation in surge tank methyl alcohol and pyridine Mixed liquor 8.1kg, first order absorption tank quantity of methyl alcohol is 1500kg, is increased weight 37.5kg after absorbing chloromethanes, and two grades of touries are The methanol aqueous solution of 400kg50%, increase weight 1.7kg after absorption chloromethanes, and three-level tourie is the clear water of 1000kg, absorbs chloromethane Increased weight 0.3kg after alkane, and active principle 47.6kg, the rate of recovery 95.20% are reclaimed altogether.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality Body or operation make a distinction with another entity or operation, and not necessarily require or imply these entities or deposited between operating In any this actual relation or order.And, term " including ", "comprising" or its any other variant be intended to Nonexcludability is included, so that process, method, article or equipment including a series of key elements not only will including those Element, but also other key elements including being not expressly set out, or also include being this process, method, article or equipment Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that Also there is other identical element in process, method, article or equipment including the key element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although with reference to the foregoing embodiments The present invention has been described in detail, it will be understood by those within the art that:It still can be to foregoing each implementation Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic;And these modification or Replace, do not make the spirit and scope of the essence disengaging various embodiments of the present invention technical scheme of appropriate technical solution.

Claims (7)

1. chloride methane waste product handling process during a kind of paraquat is produced, it is characterised in that step is as follows:By paraquat synthesis reactor The chloride methane waste product of discharge is condensed in being passed into condenser, then enters the chloromethanes equipped with gas distributor by surge tank Tourie, chimney is entered after being absorbed using three-level.
2. chloride methane waste product handling process during paraquat as claimed in claim 1 is produced, it is characterised in that the chloromethanes It is methyl alcohol that the tourie first order absorbs the absorbing liquid for using.
3. chloride methane waste product handling process during paraquat as claimed in claim 2 is produced, it is characterised in that the methyl alcohol is used It is 20-50 times of exhaust mass to measure, and treatment exhausted air quantity substitutes methyl alcohol as paraquat alkyl chemical industry after reaching the 10-30% of deadweight The solvent of section.
4. chloride methane waste product handling process during paraquat as claimed in claim 1 is produced, it is characterised in that the chloromethanes The tourie second level absorbs the absorbing liquid for using for mass fraction is the methanol aqueous solution of 50wt%.
5. chloride methane waste product handling process during paraquat as claimed in claim 4 is produced, it is characterised in that the methanol-water Solution usage is 5-10 times of exhaust mass, and methyl alcohol is substituted when methanol content reaches more than 80% in the absorbing liquid as hundred grass The solvent of withered alkylation workshop section.
6. chloride methane waste product handling process during paraquat as claimed in claim 1 is produced, it is characterised in that the chloromethanes It is water that the tourie third level absorbs the absorbing liquid for using.
7. chloride methane waste product handling process during paraquat as claimed in claim 6 is produced, it is characterised in that the use of the water It is 2-5 times of absorbing liquid quality in two grades of touries to measure, and the second level is entered when methanol content reaches more than 5% in the absorbing liquid Absorbing liquid is prepared in tourie.
CN201710005404.3A 2017-01-04 2017-01-04 Chloride methane waste product handling process in a kind of paraquat production Pending CN106823667A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108716613A (en) * 2018-05-31 2018-10-30 青岛科技大学科技公司东营分公司 Liquefied gas restoring device in the technique of ionic liquid allcylation

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108716613A (en) * 2018-05-31 2018-10-30 青岛科技大学科技公司东营分公司 Liquefied gas restoring device in the technique of ionic liquid allcylation

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Application publication date: 20170613