CN109110732A - For reducing the method for harmful substance in by-product hydrochloric acid in benzene chloride production technique - Google Patents

For reducing the method for harmful substance in by-product hydrochloric acid in benzene chloride production technique Download PDF

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Publication number
CN109110732A
CN109110732A CN201811057148.3A CN201811057148A CN109110732A CN 109110732 A CN109110732 A CN 109110732A CN 201811057148 A CN201811057148 A CN 201811057148A CN 109110732 A CN109110732 A CN 109110732A
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China
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hydrochloric acid
benzene
gas
hydrogen chloride
tower
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CN201811057148.3A
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Inventor
陈永贵
黄中桂
蔡小林
袁晓林
杨镭
王先武
罗立忠
袁树林
章子虎
张俊
丁锐
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Anhui Dongzhi Guangxin Agrochemical Co Ltd
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Anhui Dongzhi Guangxin Agrochemical Co Ltd
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Priority to CN201811057148.3A priority Critical patent/CN109110732A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/19Fluorine; Hydrogen fluoride
    • C01B7/191Hydrogen fluoride
    • C01B7/195Separation; Purification
    • C01B7/197Separation; Purification by adsorption

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention provides a kind of method in benzene chloride production technique for reducing harmful substance in by-product hydrochloric acid.The method of the present invention includes: that the normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.08-0.12MPa by roots blower, it is condensed through first-stage condenser, water and low-boiling point material are condensed, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to be forced into 1-1.5MPa by compressor, after secondary condenser condenses and further removes organic impurities, enter adsorption tower from the absorption tower bottom equipped with adsorbent, it removes other impurities and obtains qualified hydrogen chloride gas, industrial pure hydrochloric acid is obtained after water absorbs.The hydrogen chloride degree of purity that the method for the present invention obtains is high, by-product hydrochloric acid it is high-quality, waste water will not be generated, increase enterprise's income, and process flow is succinct, it is easy to operate, and the benzene series organic matter recycled from by-product hydrochloric acid enters benzene accumulator tank, it is recycled back to chloride process, reduces loss of material, reduce production cost.

Description

For reducing the method for harmful substance in by-product hydrochloric acid in benzene chloride production technique
Technical field
The present invention relates to pesticide production technology fields, and in particular to for reducing by-product in a kind of benzene chloride production technique The method of harmful substance in hydrochloric acid.
Background technique
Benzene Chloride is also chlorobenzene, is colorless and transparent volatile liquid, there is semen armeniacae amarae taste.- 45.6 DEG C of fusing point, boiling point 131.6 DEG C, relative density 1.107 (20/4 DEG C), index of refraction 1.5248 is 23 DEG C of flash-point, 637.78 DEG C of self-ignition point, inflammable.In sky Explosion limit is 1.83-9.23% (volume) in gas.It is not soluble in water, it is soluble in alcohol, ether, benzene and chloroform etc..It is toxic, in toxicity Deng.
Benzene Chloride is a kind of important basic organic synthesis raw material, is used as dyestuff, medicine, pesticide, organic synthesis intermediate. For manufacturing phenol, nitro-chlorobenzene, dinitrofluorobenzene, aniline, nitrophenols and insecticide DDT etc., ethyl cellulose is also served as With the solvent of many resins.During traditional mode of production Benzene Chloride, using benzene and chlorine under catalyst iron hoop catalyst action in Hybrid reaction is produced in chlorination reactor, contains hydrochloric acid in acid chlorization liquid after chlorination reaction, will by the methods of stripping, stripping Hydrochloric acid is changed into gaseous hydrogen chloride and takes out from chlorated liquid, then absorbs by-product hydrochloric acid, but the chlorination isolated by water The organic matters such as benzene, Benzene Chloride can be carried in hydrogen secretly makes by-product hydrochloric acid second-rate, is not able to satisfy more demanding to hydrochloric acid Production requirement.Remain in a small amount of organic matter in by-product hydrochloric acid, takes system out of with hydrochloric acid, cause wastage of material, increase life Cost is produced, while the organic matter brought into causes hidden danger in hydrochloric acid system.
Therefore, it in order to solve the problems, such as to contain the harmful substances such as benzene in benzene chloride production byproduct in process object hydrochloric acid, improves The quality of by-product hydrochloric acid is developed outstanding for reducing the method for harmful substance in by-product hydrochloric acid in a kind of benzene chloride production technique It is important.
Summary of the invention
In view of the shortcomings of the prior art, the present invention is provided in a kind of benzene chloride production technique for reducing having in by-product hydrochloric acid The method of evil substance.
In order to achieve the above object, technical solution of the present invention is achieved by the following technical programs:
For reducing the method for harmful substance in by-product hydrochloric acid in a kind of benzene chloride production technique: passing through roots blower will The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.08-0.12MPa, condenses through first-stage condenser, by water and low Boilers condensation, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to be forced into 1-1.5MPa by compressor, Enter adsorption tower from the absorption tower bottom equipped with adsorbent after secondary condenser further removes organic impurities, from overhead extraction Qualified hydrogen chloride gas, hydrogen chloride gas absorb to obtain qualified by-product hydrochloric acid to enter hydrochloric acid after cooler is cooling through absorption tower The benzene series organic matter of basin, recycling enters benzene accumulator tank, is recycled back to chloride process, and after tower adsorption saturation to be adsorbed Switch to another adsorption tower.
Further, another adsorption tower is switched to after the adsorption tower adsorption saturation, is desorbed by alternating temperature so that adsorbent Activation is applied, and is completed desorption and is recycled.
Further, the detailed process of the alternating temperature desorption are as follows: adsorption tower is inhaled in pressure 1-1.5MPa, under room temperature It is attached, after adsorption saturation, then by the adsorption tower of adsorption saturation through drop pressure three times to normal pressure, then leads to and be heated to 80 DEG C and adsorb Treated hydrogen chloride gas enters adsorption tower from tower top and carries out backwash, and the impure hydrogen chloride gas after backwash is removed through condensation It is incorporated to the hydrogen chloride gas repressurization absorption that pressure is 0.1MPa after removing organic matter, desorption is completed and is recycled.
Further, the normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.1MPa by the roots blower.
Further, the gas chlorination hydrogen continues to be forced into 1.2MPa by compressor.
The present invention provides a kind of method in benzene chloride production technique for reducing harmful substance in by-product hydrochloric acid, and existing There is technology to be compared to advantage:
For reducing the method for harmful substance in by-product hydrochloric acid in benzene chloride production technique of the present invention, tradition side is avoided Washing and alkali cleaning can lead to the problem of a large amount of waste water in method, and the method for the present invention will not generate waste water, obtain hydrogen chloride degree of purity height, Chlorination hydrogen purity >=95%, content of organics≤1000 μ g/L, the quality of by-product hydrochloric acid are improved, and obtain purification hydrochloric acid, Increase enterprise's income, and process flow is succinct, it is easy to operate, and also the benzene series organic matter recycled from by-product hydrochloric acid enters benzene Accumulator tank is recycled back to chloride process, reduces loss of material, reduces production cost;
The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.08- by roots blower by the method for the present invention 0.12MPa is condensed through first-stage condenser, and water and low-boiling point material are condensed, after being handled by gas-liquid separator separates, gas chlorine Change hydrogen to continue to be forced into 1-1.5MPa by compressor, from equipped with adsorbent after secondary condenser further removes organic impurities Absorption tower bottom enter adsorption tower, obtain qualified by-product hydrochloric acid, the benzene series organic matter of recycling enters benzene accumulator tank, return to chlorine Chemical industry sequence is recycled, and is desorbed by the adsorption tower of adsorption saturation reduction pressure to normal pressure, then by alternating temperature, completes desorption and follows Ring uses, and the method for the present invention improves the resource utilization to benzene and hydrogen chloride, economizes on resources, increase economic efficiency, Er Qieyou Sharp environment is a green technological process for practicing recycling economy development.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below with reference to the embodiment of the present invention pair Technical solution in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is a part of the invention Embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making wound Every other embodiment obtained under the premise of the property made labour, shall fall within the protection scope of the present invention.
Embodiment 1:
For reducing the method for harmful substance in by-product hydrochloric acid in the present embodiment benzene chloride production technique: passing through Roots's wind The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.08MPa by machine, is condensed through first-stage condenser, by water and low boiling Point material condensation, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to be forced into 1MPa by compressor, through second level Condenser, which further removes, enters adsorption tower from the absorption tower bottom equipped with adsorbent after organic impurities, qualified from overhead extraction Hydrogen chloride gas, hydrogen chloride gas absorb to obtain qualified by-product hydrochloric acid to enter hydrochloric acid basin after cooler is cooling through absorption tower, The benzene series organic matter of recycling enters benzene accumulator tank, is recycled back to chloride process, and switch after tower adsorption saturation to be adsorbed To another adsorption tower;Another adsorption tower is switched to after adsorption tower adsorption saturation, adsorption tower is inhaled in pressure 1MPa, under room temperature It is attached, after adsorption saturation, then by the adsorption tower of adsorption saturation through drop pressure three times to normal pressure, then leads to and be heated to 80 DEG C and adsorb Treated hydrogen chloride gas enters adsorption tower from tower top and carries out backwash, and the impure hydrogen chloride gas after backwash is removed through condensation It is incorporated to the hydrogen chloride gas repressurization absorption that pressure is 0.1MPa after removing organic matter, desorption is completed and is recycled.
Embodiment 2:
For reducing the method for harmful substance in by-product hydrochloric acid in the present embodiment benzene chloride production technique: passing through Roots's wind The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.12MPa by machine, is condensed through first-stage condenser, by water and low boiling Point material condensation, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to be forced into 1.5MPa by compressor, through two Grade condenser, which further removes, enters adsorption tower from the absorption tower bottom equipped with adsorbent after organic impurities, from overhead extraction qualification Hydrogen chloride gas, hydrogen chloride gas absorbs to obtain qualified by-product hydrochloric acid and enter hydrochloric acid after cooler is cooling through absorption tower to be store The benzene series organic matter of tank, recycling enters benzene accumulator tank, is recycled back to chloride process, and cut after tower adsorption saturation to be adsorbed Shift to another adsorption tower;Switch to another adsorption tower after adsorption tower adsorption saturation, adsorption tower in pressure 1.5MPa, under room temperature Absorption after adsorption saturation, then by the adsorption tower of adsorption saturation through drop pressure three times to normal pressure, then leads to and is heated to 80 DEG C and inhales Attached treated hydrogen chloride gas enters adsorption tower from tower top and carries out backwash, and the impure hydrogen chloride gas after backwash is through condensing It is incorporated to the hydrogen chloride gas repressurization absorption that pressure is 0.1MPa after removing organic matter, desorption is completed and is recycled.
Embodiment 3:
For reducing the method for harmful substance in by-product hydrochloric acid in the present embodiment benzene chloride production technique: passing through Roots's wind The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.1MPa by machine, is condensed through first-stage condenser, by water and low boiling Point material condensation, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to be forced into 1.2MPa by compressor, through two Grade condenser, which further removes, enters adsorption tower from the absorption tower bottom equipped with adsorbent after organic impurities, from overhead extraction qualification Hydrogen chloride gas, hydrogen chloride gas absorbs to obtain qualified by-product hydrochloric acid and enter hydrochloric acid after cooler is cooling through absorption tower to be store The benzene series organic matter of tank, recycling enters benzene accumulator tank, is recycled back to chloride process, and cut after tower adsorption saturation to be adsorbed Shift to another adsorption tower;Switch to another adsorption tower after adsorption tower adsorption saturation, adsorption tower in pressure 1.3MPa, under room temperature Absorption after adsorption saturation, then by the adsorption tower of adsorption saturation through drop pressure three times to normal pressure, then leads to and is heated to 80 DEG C and inhales Attached treated hydrogen chloride gas enters adsorption tower from tower top and carries out backwash, and the impure hydrogen chloride gas after backwash is through condensing It is incorporated to the hydrogen chloride gas repressurization absorption that pressure is 0.1MPa after removing organic matter, desorption is completed and is recycled.
Embodiment 4:
For reducing the method for harmful substance in by-product hydrochloric acid in the present embodiment benzene chloride production technique: passing through Roots's wind The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.09MPa by machine, is condensed through first-stage condenser, by water and low boiling Point material condensation, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to be forced into 1.1MPa by compressor, through two Grade condenser, which further removes, enters adsorption tower from the absorption tower bottom equipped with adsorbent after organic impurities, from overhead extraction qualification Hydrogen chloride gas, hydrogen chloride gas absorbs to obtain qualified by-product hydrochloric acid and enter hydrochloric acid after cooler is cooling through absorption tower to be store The benzene series organic matter of tank, recycling enters benzene accumulator tank, is recycled back to chloride process, and cut after tower adsorption saturation to be adsorbed Shift to another adsorption tower;Switch to another adsorption tower after adsorption tower adsorption saturation, adsorption tower in pressure 1.1MPa, under room temperature Absorption after adsorption saturation, then by the adsorption tower of adsorption saturation through drop pressure three times to normal pressure, then leads to and is heated to 80 DEG C and inhales Attached treated hydrogen chloride gas enters adsorption tower from tower top and carries out backwash, and the impure hydrogen chloride gas after backwash is through condensing It is incorporated to the hydrogen chloride gas repressurization absorption that pressure is 0.1MPa after removing organic matter, desorption is completed and is recycled.
Embodiment 5:
For reducing the method for harmful substance in by-product hydrochloric acid in the present embodiment benzene chloride production technique: passing through Roots's wind The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.11MPa by machine, is condensed through first-stage condenser, by water and low boiling Point material condensation, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to be forced into 1.4MPa by compressor, through two Grade condenser, which further removes, enters adsorption tower from the absorption tower bottom equipped with adsorbent after organic impurities, from overhead extraction qualification Hydrogen chloride gas, hydrogen chloride gas absorbs to obtain qualified by-product hydrochloric acid and enter hydrochloric acid after cooler is cooling through absorption tower to be store The benzene series organic matter of tank, recycling enters benzene accumulator tank, is recycled back to chloride process, and cut after tower adsorption saturation to be adsorbed Shift to another adsorption tower;Another adsorption tower, the detailed process of alternating temperature desorption are as follows: adsorption tower exists are switched to after adsorption tower adsorption saturation Pressure 1.4MPa, adsorb under room temperature, after adsorption saturation, then by the adsorption tower of adsorption saturation through drop pressure three times to normal Pressure, the hydrogen chloride gas then led to after being heated to 80 DEG C and adsorption treatment enters adsorption tower from tower top and carries out backwash, after backwash Impure hydrogen chloride gas is incorporated to the hydrogen chloride gas repressurization that pressure is 0.1MPa after condensation removes organic matter and adsorbs, It completes desorption and is recycled.
It should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although ginseng According to previous embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be with It modifies the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features;And These are modified or replaceed, the spirit and model of technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution It encloses.

Claims (5)

1. for reducing the method for harmful substance in by-product hydrochloric acid in a kind of benzene chloride production technique, which is characterized in that pass through The normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.08-0.12MPa by roots blower, cold through first-stage condenser It is solidifying, water and low-boiling point material are condensed, after being handled by gas-liquid separator separates, gas chlorination hydrogen continues to pressurize by compressor To 1-1.5MPa, enter absorption from the absorption tower bottom equipped with adsorbent after secondary condenser further removes organic impurities Tower, from the hydrogen chloride gas of overhead extraction qualification, hydrogen chloride gas absorbs to obtain qualified by-product hydrochloric acid through cooler through absorption tower Enter hydrochloric acid basin after cooling, the benzene series organic matter of recycling enters benzene accumulator tank, is recycled back to chloride process, and wait inhale Another adsorption tower is switched to after attached tower adsorption saturation.
2. according to claim 1 in benzene chloride production technique for reducing the method for harmful substance in by-product hydrochloric acid, It is characterized in that, another adsorption tower is switched to after the adsorption tower adsorption saturation, then be desorbed by alternating temperature, complete to be desorbed and recycling makes With.
3. according to claim 2 in benzene chloride production technique for reducing the method for harmful substance in by-product hydrochloric acid, It is characterized in that, the detailed process of the alternating temperature desorption are as follows: adsorption tower is adsorbed in pressure 1-1.5MPa, under room temperature, and absorption is full With it is rear, then by the adsorption tower of adsorption saturation through drop pressure three times to normal pressure, then lead to be heated to 80 DEG C and adsorption treatment after Hydrogen chloride gas enters adsorption tower from tower top and carries out backwash, and the impure hydrogen chloride gas after backwash removes organic matter through condensation It is incorporated to the hydrogen chloride gas repressurization that pressure is 0.1MPa afterwards to adsorb, completes desorption and is recycled.
4. according to claim 1 in benzene chloride production technique for reducing the method for harmful substance in by-product hydrochloric acid, It is characterized in that, the normal pressure hydrogen chloride gas that Benzene Chloride system is isolated is forced into 0.1MPa by the roots blower.
5. according to claim 1 in benzene chloride production technique for reducing the method for harmful substance in by-product hydrochloric acid, It is characterized in that, the gas chlorination hydrogen continues to be forced into 1.2MPa by compressor.
CN201811057148.3A 2018-09-11 2018-09-11 For reducing the method for harmful substance in by-product hydrochloric acid in benzene chloride production technique Pending CN109110732A (en)

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CN115417381A (en) * 2022-09-06 2022-12-02 江苏瑞祥化工有限公司 Method for recycling byproduct hydrochloric acid containing machine components
CN116812871A (en) * 2022-12-08 2023-09-29 山东赛斯特冷冻系统有限公司 Process and equipment for preparing high-purity hydrogen chloride from byproduct tail gas of chlorotoluene production

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CN101448738A (en) * 2006-05-12 2009-06-03 拜尔材料科学股份公司 Improved Process for Purification of Anhydrous Hydrogen Chloride Gas
CN1951801A (en) * 2006-06-15 2007-04-25 浙江工业大学 Process for preparing high purity hydrochloric acid by circularly absorbing hydrogen chloride by-product
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Publication number Priority date Publication date Assignee Title
CN115417381A (en) * 2022-09-06 2022-12-02 江苏瑞祥化工有限公司 Method for recycling byproduct hydrochloric acid containing machine components
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CN116812871A (en) * 2022-12-08 2023-09-29 山东赛斯特冷冻系统有限公司 Process and equipment for preparing high-purity hydrogen chloride from byproduct tail gas of chlorotoluene production

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