CN111359401A - Method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas - Google Patents
Method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas Download PDFInfo
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- CN111359401A CN111359401A CN202010192978.8A CN202010192978A CN111359401A CN 111359401 A CN111359401 A CN 111359401A CN 202010192978 A CN202010192978 A CN 202010192978A CN 111359401 A CN111359401 A CN 111359401A
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- -1 amine salt Chemical class 0.000 title claims abstract description 50
- TVLSRXXIMLFWEO-UHFFFAOYSA-N prochloraz Chemical compound C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl TVLSRXXIMLFWEO-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000005820 Prochloraz Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 35
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 61
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000005917 acylation reaction Methods 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000011552 falling film Substances 0.000 claims abstract description 17
- 238000010521 absorption reaction Methods 0.000 claims abstract description 16
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 15
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 230000006378 damage Effects 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 59
- 230000010933 acylation Effects 0.000 claims description 12
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 10
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 239000002912 waste gas Substances 0.000 abstract description 2
- 238000005576 amination reaction Methods 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- LINPIYWFGCPVIE-UHFFFAOYSA-N 2,4,6-trichlorophenol Chemical compound OC1=C(Cl)C=C(Cl)C=C1Cl LINPIYWFGCPVIE-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- LAYPMCGIWDGYKX-UHFFFAOYSA-N trichloromethyl hydrogen carbonate Chemical compound OC(=O)OC(Cl)(Cl)Cl LAYPMCGIWDGYKX-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004464 cereal grain Substances 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- UCPYLLCMEDAXFR-UHFFFAOYSA-N triphosgene Chemical compound ClC(Cl)(Cl)OC(=O)OC(Cl)(Cl)Cl UCPYLLCMEDAXFR-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/75—Multi-step processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/005—Separation 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 heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/14—Separation 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
- B01D53/1406—Multiple stage absorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/14—Separation 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
- B01D53/1456—Removing acid components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/08—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions not involving the formation of amino groups, hydroxy groups or etherified or esterified hydroxy groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
- B01D2252/103—Water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/20—Organic absorbents
- B01D2252/205—Other organic compounds not covered by B01D2252/00 - B01D2252/20494
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Abstract
The invention belongs to the technical field of tail gas treatment, and particularly relates to a method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas, which comprises the following steps: (1) introducing acid tail gas generated by prochloraz acylation reaction into an organic solution of an aminated substance at the temperature of-5-45 ℃ to enable hydrogen chloride in the acid tail gas to react with the aminated substance to generate amine salt, and controlling the pH value to be 1-5 at the end of the reaction; (2) sequentially carrying out primary falling film absorption and secondary falling film absorption treatment on the acid tail gas remaining after the reaction in the step (1) at the temperature of-10-30 ℃; (3) and (3) treating the residual acid tail gas treated in the step (2) by a phosgene destruction tower, absorbing by alkali liquor, and then discharging at high altitude. The method changes the tail gas in the acylation reaction process for producing the prochloraz into valuable, recycles the waste gas, can reduce the production cost of the prochloraz, can reduce the load and cost of environmental protection treatment, and effectively improves the environmental safety.
Description
Technical Field
The invention belongs to the technical field of tail gas treatment, and particularly relates to a method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas.
Background
Prochloraz (Prochloraz), the chemical name of which is N-propyl-N- (2, 4, 6-trichlorophenoxyethyl) -1H-imidazole-1-formamide, is an imidazole high falsehood broad-spectrum bactericide which is synthesized in 1974 of BootsCo.A. in UK, Ltd, and marketed in 1977, acts by inhibiting the biosynthesis of sterol, and has good control effect on various germs of rice, fruits and cereal grains.
At present, domestic manufacturers adopt methods of etherifying 2, 4, 6-trichlorophenol and dichloroethane in sodium hydroxide, amination, acyl chlorination and condensation to produce prochloraz, the production processes are basically the same, and the process flow is as follows: taking 2, 4, 6-trichlorophenol as a starting material, adding liquid alkali for dissolving, and then carrying out pressure etherification with dichloroethane; washing with water to remove dichloroethane; refluxing and aminating in propylamine, reinforcing alkali after aminating, steaming to remove propylamine, cooling, and adding hydrochloric acid to obtain secondary amine salt precipitate; filtering to separate insoluble substance, dehydrating the filter cake with toluene, and adding trichloromethyl carbonate (BTC) for acyl chlorination; then condensing with imidazole in the presence of triethylamine; and washing and refining the condensation solution, and removing toluene in an organic layer in vacuum to obtain the prochloraz original drug.
However, triphosgene or phosgene is used as a chlorinating agent in the acylation process, and a large amount of acidic tail gas (hydrogen chloride gas, a small amount of toluene and a small amount of phosgene) is generated in the chlorination process. According to the prochloraz preparation process reported in the prior art, hydrogen chloride in part of tail gas is directly neutralized by liquid alkali by a manufacturer, and hydrogen chloride in part of tail gas is absorbed by falling film firstly and then is changed into waste hydrochloric acid and then is treated as hazardous waste by the manufacturer.
Disclosure of Invention
The invention aims to solve the problems, and provides a method for co-producing amine salt by utilizing prochloraz acylation acidic tail gas, which changes the tail gas in prochloraz acylation reaction into valuable, recycles the waste, reduces the production cost of prochloraz, reduces the load of environmental protection treatment and improves the safety performance of environmental protection.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas comprises the following steps:
(1) introducing acid tail gas generated by prochloraz acylation reaction into an organic solution of an aminated substance at the temperature of-5-45 ℃ to enable hydrogen chloride in the acid tail gas to react with the aminated substance to generate amine salt, and controlling the pH value to be 1-5 at the end of the reaction;
(2) sequentially carrying out primary falling film absorption and secondary falling film absorption treatment on the acid tail gas remaining after the reaction in the step (1) at the temperature of-10-30 ℃;
(3) and (3) treating the residual acid tail gas treated in the step (2) by a phosgene destruction tower, absorbing by alkali liquor, and then discharging at high altitude.
Preferably, the volume content of hydrogen chloride, toluene and phosgene in the acidic tail gas generated by the prochloraz acylation reaction is 87-95%, 6-12% and 0.01-1%.
Preferably, the mass-volume ratio of the amine compound to the organic solution is (2-8): 1.
Preferably, the organic solution is selected from one of toluene, xylene or chlorobenzene.
Preferably, in the step (1), the acidic tail gas generated by the acylation reaction of prochloraz is introduced into the toluene solution of aminated substance at the temperature of 5-30 ℃.
Preferably, in the step (1), the reaction end point controls the pH value to be 3-4.
Preferably, in the step (2), the acidic tail gas remaining after the reaction in the step (1) is subjected to primary falling film absorption and secondary falling film absorption in sequence at a temperature of-10 ℃ to 5 ℃.
Preferably, the solvent used in the first-stage falling film absorption and the second-stage falling film absorption is one selected from toluene, dichloroethane, chlorobenzene or tap water.
The principle of the method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas is as follows:
amine salt (amide hydrochloride, see equation 1) reacts with phosgene (one molecule of solid phosgene decomposes into three molecules of phosgene, see equation 2) to form an acylate, two molecules of hydrogen chloride are released (see equation 3), the tail gas of the acylation reaction mainly contains a large amount of hydrogen chloride gas, the tail gas can be used for an amine salt forming process, so that most of hydrogen chloride and amine react to generate amine salt (see equation 1), the rest small amount of unabsorbed hydrogen chloride is converted into hydrochloric acid through primary falling film absorption and secondary falling film absorption, trace phosgene after falling film absorption is treated through a phosgene destruction tower, trace hydrogen chloride is completely absorbed and destroyed through a liquid alkali spray tower, and a small amount of toluene is consumed in the process of reacting hydrogen chloride and amine to generate amine salt, so that the discharged tail gas does not contain any harmful components.
Compared with the prior art, the invention has the following advantages and positive effects:
the method has the advantages that tail gas in the acylation reaction process for producing the prochloraz can be changed into valuable, the waste gas is recycled, the production cost of the prochloraz can be reduced, the environmental protection treatment load can be reduced, the environmental protection treatment cost can be reduced, and the environmental safety can be effectively improved. Specifically, a large amount of hydrogen chloride gas in the prochloraz acylation acidic tail gas is recycled, toxic and harmful substances in the tail gas are removed, and the pollution to the environment is reduced; reduce the treatment cost of the byproduct hydrochloric acid (the prior art needs to pay the other side 100 yuan/ton on average when the byproduct hydrochloric acid is handed to the unit with the treatment qualification of the waste hydrochloric acid).
Drawings
FIG. 1 is a schematic diagram of the process for treating and recycling the acylation tail gas in the prochloraz production process.
Detailed Description
The following detailed description of specific embodiments of the invention refers to the accompanying drawings.
Comparative example 1
Preparing a toluene solution of an aminated substance in advance in an amination salifying kettle (the mass volume ratio of the aminated substance to the toluene is 5:1), starting stirring, controlling the kettle temperature to be within the range of 15-25 ℃, dropwise adding 30% of industrial hydrochloric acid into the salifying kettle, observing the online pH meter of the amine salt forming kettle, stopping dropwise adding the hydrochloric acid when the pH value reaches 3-4, and carrying out subsequent procedures on the amine salt to obtain white wet amine salt, wherein the content of the amine salt is 92.5%, and the yield is 85.3%.
Example 1
Preparing a toluene solution of an aminated substance in advance in an amination salifying kettle (the mass volume ratio of the aminated substance to the toluene is 5:1), starting stirring, controlling the kettle temperature to be within the range of 15-25 ℃, introducing prochloraz acylation acidic tail gas into an amine salt forming kettle through a buffer tank, observing an online pH meter of the amine salt forming kettle in the process of introducing the acidic tail gas, gradually and slowly reducing the pH value from 10, stopping introducing the tail gas when the pH value reaches 3-4, and performing subsequent processes on the amine salt to obtain white wet amine salt, wherein the content of the amine salt is 99.8%, and the yield is 96.7%.
Example 2
Preparing a toluene solution of an aminated substance in advance in an amination salifying kettle (the mass volume ratio of the aminated substance to the toluene is 3:1), starting stirring, controlling the kettle temperature to be within the range of 15-25 ℃, introducing prochloraz acylation acidic tail gas into an amine salt forming kettle through a buffer tank, observing an online pH meter of the amine salt forming kettle in the process of introducing the acidic tail gas, gradually and slowly reducing the pH value from 10, stopping introducing the tail gas when the pH value reaches 1-2, and performing subsequent processes on the amine salt to obtain white wet amine salt, wherein the content of the amine salt is 99.6%, and the yield is 96.5%.
Example 3
Preparing a dimethylbenzene solution of an aminate in advance in an amination salifying kettle (the mass volume ratio of the aminate to methylbenzene is 6:1), starting stirring, controlling the kettle temperature to be within the range of 15-25 ℃, introducing prochloraz acylation acidic tail gas into an amine salt forming kettle through a buffer tank, observing an online pH meter of the amine salt forming kettle in the process of introducing the acidic tail gas, gradually and slowly reducing the pH value from 10, stopping introducing the tail gas when the pH value reaches 3-4, and performing subsequent processes on the amine salt to obtain white wet amine salt, wherein the content of the amine salt is 99.7%, and the yield is 96.6%.
Example 4
Preparing a chlorobenzene solution of an aminated substance in advance in an amination salifying kettle (the mass volume ratio of the aminated substance to toluene is 7:1), starting stirring, controlling the kettle temperature to be within the range of 15-25 ℃, introducing prochloraz acylation acidic tail gas into an amine salt forming kettle through a buffer tank, observing an online pH meter of the amine salt forming kettle in the process of introducing the acidic tail gas, gradually and slowly reducing the pH value from 10, stopping introducing the tail gas when the pH value reaches 3-4, and performing subsequent processes on the amine salt to obtain white wet amine salt, wherein the content of the amine salt is 99.6%, and the yield is 96.6%.
The above embodiments are merely preferred embodiments of the present invention, and any simple modification, modification and substitution changes made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (8)
1. A method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas is characterized by comprising the following steps:
(1) introducing acid tail gas generated by prochloraz acylation reaction into an organic solution of an aminated substance at the temperature of-5-45 ℃ to enable hydrogen chloride in the acid tail gas to react with the aminated substance to generate amine salt, and controlling the pH value to be 1-5 at the end of the reaction;
(2) sequentially carrying out primary falling film absorption and secondary falling film absorption treatment on the acid tail gas remaining after the reaction in the step (1) at the temperature of-10-30 ℃;
(3) and (3) treating the residual acid tail gas treated in the step (2) by a phosgene destruction tower, absorbing by alkali liquor, and then discharging at high altitude.
2. The method for co-production of amine salt by utilizing prochloraz acylation acidic tail gas as claimed in claim 1, wherein the acidic tail gas generated by prochloraz acylation reaction contains 87-95% by volume of hydrogen chloride, 6-12% by volume of toluene and 0.01-1% by volume of phosgene.
3. The method for co-production of amine salt by using prochloraz acylated acidic tail gas as claimed in claim 1, wherein the mass volume ratio of the amine compound to the organic solution is (2-8): 1.
4. The method for co-production of amine salt by acylation of acidic exhaust gas with prochloraz according to claim 1 or 3, wherein the organic solution is selected from one of toluene, xylene or chlorobenzene.
5. The method for co-production of amine salt by utilizing prochloraz acylation acidic tail gas as claimed in claim 4, wherein in the step (1), the acidic tail gas generated by prochloraz acylation reaction is introduced into toluene solution of aminated substance at the temperature of 5-30 ℃.
6. The method for co-producing amine salt by acylating acidic tail gas with prochloraz according to claim 1, wherein in the step (1), the pH is controlled to be 3-4 at the end of the reaction.
7. The method for co-producing amine salt by utilizing prochloraz acylated acidic tail gas according to claim 1, wherein in the step (2), the acidic tail gas remained after the reaction in the step (1) is subjected to primary falling film absorption and secondary falling film absorption sequentially at a temperature of-10 ℃ to 5 ℃.
8. The method for co-production of amine salt by acylation of acidic tail gas with prochloraz according to claim 1 or 7, wherein the solvent used in the first and second falling film absorption is selected from one of toluene, dichloroethane, chlorobenzene or tap water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115850118A (en) * | 2022-12-26 | 2023-03-28 | 江西汇和化工有限公司 | Continuous synthesis method of prochloraz intermediate |
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| CN101348252A (en) * | 2008-04-25 | 2009-01-21 | 甘肃银光化学工业集团有限公司 | Phosgene recovery method for toluene diisocyanate production process |
| CN101402608A (en) * | 2008-11-25 | 2009-04-08 | 乐斯化学有限公司 | Method for producing bactericide prochloraz |
| CN103638688A (en) * | 2013-12-24 | 2014-03-19 | 湖南国发精细化工科技有限公司 | Recycling method for phosgene in tail gas generated in calorescence reaction for synthesizing normal-butyl isocyanate |
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