CN112830875A - Method and system for recycling acid wastewater and rectification residual liquid in trichloro-acetic chloride production process - Google Patents
Method and system for recycling acid wastewater and rectification residual liquid in trichloro-acetic chloride production process Download PDFInfo
- Publication number
- CN112830875A CN112830875A CN202110018989.9A CN202110018989A CN112830875A CN 112830875 A CN112830875 A CN 112830875A CN 202110018989 A CN202110018989 A CN 202110018989A CN 112830875 A CN112830875 A CN 112830875A
- Authority
- CN
- China
- Prior art keywords
- kettle
- recycling
- chlorination
- residual liquid
- outlet
- Prior art date
- 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
Links
- 238000004064 recycling Methods 0.000 title claims abstract description 159
- 239000007788 liquid Substances 0.000 title claims abstract description 104
- PVFOMCVHYWHZJE-UHFFFAOYSA-N trichloroacetyl chloride Chemical compound ClC(=O)C(Cl)(Cl)Cl PVFOMCVHYWHZJE-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000002351 wastewater Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002253 acid Substances 0.000 title claims description 15
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 158
- 230000007062 hydrolysis Effects 0.000 claims abstract description 78
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000047 product Substances 0.000 claims abstract description 39
- 239000011265 semifinished product Substances 0.000 claims abstract description 37
- 238000011084 recovery Methods 0.000 claims abstract description 27
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000460 chlorine Substances 0.000 claims abstract description 25
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 25
- 230000002378 acidificating effect Effects 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 13
- VGCXGMAHQTYDJK-UHFFFAOYSA-N Chloroacetyl chloride Chemical compound ClCC(Cl)=O VGCXGMAHQTYDJK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- FBCCMZVIWNDFMO-UHFFFAOYSA-N dichloroacetyl chloride Chemical compound ClC(Cl)C(Cl)=O FBCCMZVIWNDFMO-UHFFFAOYSA-N 0.000 claims abstract description 10
- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012346 acetyl chloride Substances 0.000 claims abstract description 9
- 238000007670 refining Methods 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims description 53
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 46
- 238000009833 condensation Methods 0.000 claims description 46
- 230000005494 condensation Effects 0.000 claims description 46
- 229940106681 chloroacetic acid Drugs 0.000 claims description 38
- 239000012452 mother liquor Substances 0.000 claims description 38
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 23
- 229910052717 sulfur Inorganic materials 0.000 claims description 23
- 239000011593 sulfur Substances 0.000 claims description 23
- 238000007599 discharging Methods 0.000 claims description 21
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 14
- 150000001263 acyl chlorides Chemical class 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims 6
- 150000002019 disulfides Chemical class 0.000 claims 3
- 238000005086 pumping Methods 0.000 claims 2
- 239000007792 gaseous phase Substances 0.000 claims 1
- 239000002699 waste material Substances 0.000 claims 1
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 208000005156 Dehydration Diseases 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 125000004119 disulfanediyl group Chemical group *SS* 0.000 description 1
- PXJJSXABGXMUSU-UHFFFAOYSA-N disulfur dichloride Chemical compound ClSSCl PXJJSXABGXMUSU-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/62—Preparation of carboxylic acid halides by reactions not involving the carboxylic acid halide group
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/64—Separation; Purification; Stabilisation; Use of additives
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The method for recycling the acidic wastewater and the rectification residual liquid in the trichloroacetyl chloride production process comprises the following steps: adding a catalyst into the recovery chlorination kettle; introducing chlorine into the chlorination kettle to react acetyl chloride, monochloroacetic chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride; condensing and collecting light component products of the reaction of the recycling chlorination kettle to a recycling semi-finished product tank, then sending to a trichloroacetyl chloride secondary rectifying tower for refining to obtain a trichloroacetyl chloride product, and sending heavy component residual liquid in the recycling chlorination kettle to a hydrolysis kettle; the method comprises the steps of introducing water into a hydrolysis kettle to hydrolyze heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water.
Description
Technical Field
The invention relates to the technical field of preparation of acid chloride-containing substances, in particular to a method and a system for recycling acid wastewater and rectification residual liquid in a trichloro-acetic chloride production process.
Background
The liquid is colorless, transparent and easy to flow, has pungent smell, and is fuming when meeting humid air. Boiling point of 118-120 deg.C (0.1MPa), density of 1.6329(20/4 deg.C), and refractive index nD1.4700. Has strong irritation and corrosivity, and can burn skin, irritate mucosa, and corrode metal. It is insoluble in water, but can be decomposed violently by hot water to generate trichloroacetic acid and hydrogen chloride, which are dissolved in most organic solvents but decomposed by lower alcohol.
When chloroacetic acid mother liquor is used as a raw material for trichloroacetyl chloride production, water cannot be contained in the chloroacetic acid mother liquor, separate dehydration treatment is needed before use, acid wastewater after dehydration cannot be recycled and can only be used for wastewater treatment, meanwhile, the chloroacetic acid mother liquor process belongs to an advanced chlorination process, a byproduct generated in the reaction process has a high boiling point, enters rectification residual liquor in the primary rectification process and the secondary rectification process and is separated, the residual liquor is generated from dozens of tons to hundreds of tons, oil-mixed reaction intermediates in the rectification residual liquor, such as acetyl chloride, monochloroacetyl chloride, dichloroacetyl chloride and partial trichloroacetyl chloride, have active reactivity, and react violently when meeting water, and the storage risk and the treatment difficulty of the intermediates become troublesome problems for enterprises.
In the prior art, only acidic wastewater and rectification raffinate produced by chloroacetic acid mother liquor can be transferred to a chemical waste treatment station for treatment, so that raw materials and products are wasted, the treatment cost is high, the treatment difficulty is high, and serious potential safety hazards and environmental risks exist in the transferring, storing, transporting and treating processes.
Disclosure of Invention
There is a need for a method for recycling acidic wastewater and rectification raffinate in the production process of trichloroacetyl chloride.
A method for recycling acid wastewater and rectification residual liquid in the production process of trichloroacetyl chloride comprises the following steps:
adding a catalyst into the recovery chlorination kettle;
metering and vacuumizing the rectification residual liquid generated in the production process of trichloroacetyl chloride to a recovery chlorination kettle;
heating the recycling chlorination kettle to a preset temperature; introducing chlorine to react acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride;
condensing and collecting light component products of the reaction of the recycling chlorination kettle to a recycling semi-finished product tank, then sending to a trichloroacetyl chloride secondary rectifying tower for refining to obtain a trichloroacetyl chloride product, and sending heavy component residual liquid in the recycling chlorination kettle to a hydrolysis kettle;
and introducing water into the hydrolysis kettle to hydrolyze the heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water.
A system for recycling acid wastewater and rectification raffinate in trichloroacetyl chloride production process comprises a recycling chlorination kettle, a hydrolysis kettle and a centrifugal machine, wherein the recycling chlorination kettle is provided with an inlet for introducing chlorine, an inlet for introducing rectification raffinate, an inlet for adding a catalyst and an outlet for discharging heavy component raffinate, a recycling condenser and a recycling condensation receiving tank are also arranged above the recycling chlorination kettle, a tower top gas phase outlet of the recycling chlorination kettle is connected with the recycling condenser, a first backflow port of the recycling condenser is connected with the recycling chlorination kettle, a second backflow port of the recycling condenser is connected with the recycling condensation receiving tank, an outlet of the recycling condensation receiving tank is connected with a recycling semi-finished product tank, a heavy component raffinate outlet of the recycling chlorination kettle is connected with the hydrolysis kettle, the hydrolysis kettle is provided with an inlet for introducing absorption water, an inlet for adding heavy component raffinate is arranged in the hydrolysis kettle, and a stirring mechanism is arranged in the hydrolysis kettle, the hydrolysis kettle is further provided with an outlet for discharging residual liquid, the outlet of the hydrolysis kettle is connected with a centrifugal machine, the centrifugal machine is provided with a fixed residue outlet and a condensate outlet, and a condensate outlet is connected with a condensate buffer tank.
In the invention, chloroacetic acid mother liquor is separated and treated, dehydrated mother liquor is recycled to deep trichloroacetyl chloride, acid waste water is used for absorbing residual liquor, the rectified residual liquor is subjected to secondary deep chlorination reaction, acyl chloride components in the rectified residual liquor are fully absorbed and converted into trichloroacetyl chloride, heavy components in the residual liquor are centrifuged into solid impurities, active components are not contained in the heavy components, and the heavy components are stored safely, reliably and dangerously, and liquid waste is converted into a solid state, so that the heavy components are convenient to store.
Drawings
FIG. 1 is a schematic diagram of a first preferred embodiment of the present invention.
FIG. 2 is a schematic diagram of a second preferred embodiment of the present invention.
FIG. 3 is a schematic diagram of a third preferred embodiment of the present invention.
FIG. 4 is a schematic diagram of a fourth preferred embodiment of the present invention.
In the figure: the device comprises a vulcanizing kettle 10, a primary chlorination kettle 20, a primary rectifying tower 30, a primary condenser 31, a primary condensation receiving tank 32, a semi-finished product kettle 40, a secondary chlorination kettle 50, a secondary rectifying tower 60, a finished product kettle 70, a recovery chlorination kettle 80, a recovery condenser 81, a recovery condensation receiving tank 82, a hydrolysis kettle 90, a centrifuge 100, a distillation kettle 200, a distillation condenser 201 and a distillation condensation receiving tank 202.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
The embodiment of the invention provides a method for recycling acidic wastewater and rectification residual liquid in a trichloroacetyl chloride production process, which comprises the following steps:
adding catalyst (in the preferred embodiment, sulfur and/or pyridine) to the recycle chlorination reactor 80;
metering and vacuumizing the rectification residual liquid generated in the production process of trichloroacetyl chloride into a recovery chlorination kettle 80;
heating the recovered chlorination kettle 80 to a preset temperature (the preset temperature can be 110 ℃), and introducing chlorine gas to react acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride;
condensing and collecting light component products reacted in the recycling chlorination kettle 80 to a recycling semi-finished product tank, then sending the light component products to a trichloroacetyl chloride secondary rectifying tower 60 for refining to obtain trichloroacetyl chloride products, and sending heavy component residual liquid in the recycling chlorination kettle 80 to a hydrolysis kettle 90;
and (3) introducing water into the hydrolysis kettle 90 to hydrolyze the heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water. See fig. 1.
In the scheme, the rectification residual liquid is introduced into a chlorination recovery kettle 80 for reaction and absorption once, and the acid chloride in the residual liquid is fully reacted and converted into trichloro-acetyl chloride, so that the acid chloride is completely reacted and absorbed; the generated trichloro-acetyl chloride is condensed and collected to be refined, the heavy component residual liquid is hydrolyzed for secondary treatment, the heavy component impurities are independently made into fixed residues through centrifugation after hydrolysis, and the hydrolysis product is converted into condensed water for recycling. The scheme fully converts the chloracyl contained in the rectification residual liquid into trichloro-acetyl chloride for refining, converts the impurities which cannot be utilized into fixed residues, is convenient for centralized collection and disposal, more importantly, the acyl chloride components with strong activity, such as trichloro-acetyl chloride, contained in the solid residues are hydrolyzed, absorbed and centrifugally separated, so that no active substance exists in the fixed residues, the space is saved by storage, the performance of the substance is stable after storage, and no safety accident occurs when the substance meets water and is easy to explode.
This scheme still sets up the condenser for retrieving chlorination cauldron 80, continues to let in chlorine, observes the state of reflux, when no reaction solution backward flow, stops to let in chlorine. The excess chlorine gas is used to ensure that all the acid chloride contained in the solution reacts to generate trichloroacetyl chloride.
Further, in the method, in the step of introducing water into the hydrolysis kettle 90 to hydrolyze the heavy component residual liquid and performing centrifugal separation to obtain solid residue and condensed water, the acidic wastewater in the chloroacetic acid mother liquor is utilized by the water level introduced into the hydrolysis kettle 90.
Further, the acid wastewater is derived from chloroacetic acid mother liquor generated in the system, the chloroacetic acid mother liquor is injected into a recovery distillation still 200 for distillation and separation, the separated dehydrated chloroacetic acid mother liquor is used as a raw material for trichloroacetyl chloride production, and the separated acid wastewater is sent into a hydrolysis still 90 for hydrolysis of heavy component residual liquid. See fig. 2.
As the raw material for trichloroacetyl chloride production needs chloroacetic acid mother liquor, in the original production, pure anhydrous chloroacetic acid mother liquor is purchased as the raw material, or the existing chloroacetic acid mother liquor is subjected to dehydration and separation, the separation process not only increases the production period and equipment investment, but also the acid wastewater obtained after separation needs to be treated separately. The chloroacetic acid mother liquor is subjected to distillation separation in the scheme, so that not only is the dehydrated chloroacetic acid mother liquor obtained and used as a raw material, but also the acidic wastewater is not required to be treated independently and can be used as water absorbed by the hydrolysis kettle 90, the component residual liquid is subjected to hydrolysis treatment, the additional utilization value of the acidic wastewater is improved, and the environmental protection pressure of subsequent treatment of the acidic wastewater is reduced.
Further, the method for recovering the rectification residual liquid and the acidic waste water is applied to a trichloroacetyl chloride production method, and is combined with the trichloroacetyl chloride production method to form a trichloroacetyl chloride production method with the recovery and utilization values of the acidic waste water and the rectification residual liquid, and the method comprises the following steps:
introducing chlorine and sulfur into the vulcanizing kettle to produce disulfide dichloride;
introducing dithio dichloride, chlorine and chloroacetic acid mother liquor into the primary chlorination kettle 20, and preparing an acyl chloride mixture through primary chlorination; (after primary chlorination, the mixture of the acyl chloride at least contains 30-50% of monochloroacetic chloride, 30-50% of dichloroacetyl chloride and 10-20% of trichloroacetyl chloride);
the product after primary chlorination is rectified for the first time, the rectified light component is condensed and collected to a semi-finished product kettle 40, and the heavy component forms primary rectification residual liquid;
introducing chlorine and a catalyst into the secondary chlorination kettle 50, and conveying the substances in the semi-finished product kettle 40 into the secondary chlorination kettle 50 for secondary chlorination reaction;
secondarily rectifying the product prepared by secondary chlorination, condensing and collecting the rectified light component to a finished product kettle 70, and forming secondary rectification residual liquid by the heavy component;
adding catalyst (in the preferred embodiment, sulfur and/or pyridine) to the recycle chlorination reactor 80;
metering and vacuumizing the primary rectification residual liquid and the secondary rectification residual liquid to a recovery chlorination kettle 80;
heating the recovered chlorination kettle 80 to a preset temperature (the preset temperature can be 110 ℃), and introducing chlorine gas to react acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride;
condensing and collecting light component products reacted in the recycling chlorination kettle 80 to a recycling semi-finished product tank, sending to a secondary rectifying tower 60 for secondary rectification to obtain trichloroacetyl chloride products, and sending heavy component residual liquid in the recycling chlorination kettle 80 to a hydrolysis kettle 90;
and (3) introducing water into the hydrolysis kettle 90 to hydrolyze the heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water. See fig. 3.
Further, in the production process of trichloroacetyl chloride, in the step of introducing water into the hydrolysis kettle 90 to hydrolyze the heavy component residual liquid and performing centrifugal separation to obtain solid residue and condensed water, the water level introduced into the hydrolysis kettle 90 utilizes the acidic wastewater in the chloroacetic acid mother liquor.
Further, the acid wastewater is from chloroacetic acid mother liquor treatment, i.e. chloroacetic acid mother liquor is injected into a recovery distillation still 200 for distillation and separation, the separated dehydrated chloroacetic acid mother liquor is sent to a primary chlorination still 20 to be used as a raw material for trichloroacetyl chloride production, and the separated acid wastewater is sent to a hydrolysis still 90 to be used for hydrolyzing heavy component residual liquid. See fig. 4.
In the scheme, the acidic wastewater and the twice-rectified raffinate in the chloroacetic acid mother liquor are recycled and reused in the system, so that the hazardous waste discharge pressure and the subsequent treatment pressure are greatly reduced, valuable substances are recycled and converted into trichloro-acetyl chloride substances, and the substance conversion rate is improved.
The invention also provides a recycling system of acid wastewater and rectification raffinate in the production process of trichloroacetyl chloride, which comprises a recycling chlorination kettle 80, a hydrolysis kettle 90 and a centrifuge 100, wherein the recycling chlorination kettle 80 is provided with an inlet for introducing chlorine, an inlet for introducing rectification raffinate, an inlet for adding a catalyst and an outlet for discharging heavy component raffinate, a recycling condenser 81 and a recycling condensation receiving tank 82 are also arranged above the recycling chlorination kettle 80, a gas phase outlet at the top of the recycling chlorination kettle is connected with the recycling condenser 81, a first return port of the recycling condenser 81 is connected with the recycling chlorination kettle 80, a second return port of the recycling condenser 81 is connected with the recycling condensation receiving tank 82, an outlet of the recycling condensation receiving tank 82 is connected with a recycling semi-finished product tank, a heavy component raffinate outlet of the recycling chlorination kettle 80 is connected with the hydrolysis kettle 90, the hydrolysis kettle 90 is provided with an inlet for introducing absorption water, and a raffinate inlet for adding heavy components, the inside rabbling mechanism that sets up of cauldron 90 hydrolysises, and cauldron 90 hydrolysises still sets up the export of discharge raffinate, and cauldron 90 hydrolysises's exit linkage centrifuge 100, and centrifuge 100 sets up fixed residue export and comdenstion water export, comdenstion water exit linkage comdenstion water buffer tank.
The return temperature of the first return port is lower than the return temperature of the second return port. This is achievable in existing designs of condensers.
Further, still set up the metering tank at recovery chlorination cauldron 80 top, the metering tank sets up the entry of adding the rectification raffinate, and the export of metering tank is connected with recovery chlorination cauldron 80.
Further, the recycling system further comprises a distillation still 200, the distillation still 200 is provided with an inlet for introducing chloroacetic acid mother liquor, an outlet for discharging dehydrated chloroacetic acid is provided, a distillation condenser 201 and a distillation condensation receiving tank 202 are further arranged above the distillation still 200, a tower top gas phase outlet of the distillation chlorination still is connected with the distillation condenser 201, a first reflux port of the distillation condenser 201 is connected with the distillation still 200, a second reflux port of the distillation condenser 201 is connected with the distillation condensation receiving tank 202, and an outlet of the distillation condensation receiving tank 202 is connected with an inlet for introducing absorption water for the hydrolysis kettle 90, so that chloroacetic acid wastewater is introduced into the hydrolysis kettle 90.
Further, the recycling system comprises a sulfur melting kettle 10, a primary chlorination kettle 20, a primary rectifying tower 30, a semi-finished product kettle 40, a secondary chlorination kettle 50, a secondary rectifying tower 60, a finished product kettle 70, a recycling chlorination kettle 80, a hydrolysis kettle 90 and a centrifuge 100, wherein the sulfur melting kettle 10 is provided with an inlet for introducing chlorine gas, an inlet for adding sulfur and a discharge port, the discharge port of the sulfur melting kettle 10 is connected with a disulfur dichloride inlet of the primary chlorination kettle 20, the primary chlorination kettle 20 is also provided with an inlet for introducing chlorine gas, an inlet for introducing chloroacetic acid mother liquor and an outlet for discharging acyl chloride-containing mixture, an outlet of the chlorination kettle is connected with the primary rectifying tower 30 in sequence, the primary rectifying tower 30 is provided with a gas phase outlet at the top of the tower, a reflux port and a residual liquid outlet of the tower kettle, a primary condenser 31 and a primary condensation receiving groove 32 are arranged above the primary rectifying tower 30, the primary condenser 31 is used for refluxing acyl chloride-containing mixture to, the heavy component residual liquid is refluxed into the primary rectifying tower 30, an outlet of the primary condensation receiving tank 32 is connected with the semi-finished product kettle 40, an outlet of the semi-finished product kettle 40 is connected with an inlet of the secondary chlorination kettle 50, the secondary chlorination kettle 50 is provided with an inlet for introducing chlorine gas, an inlet for adding catalyst and an outlet, an outlet of the secondary chlorination kettle 50 is connected with an inlet of the secondary rectifying tower 60, the secondary rectifying tower 60 is provided with a recovery inlet, a light component outlet at the top of the tower and a residual liquid outlet at the bottom of the tower, and the finished product kettle 70 is connected with the light component substances condensed by the secondary rectifying tower 60; the recycling chlorination kettle 80 is provided with an inlet for introducing chlorine, an inlet for introducing rectification residual liquid, an inlet for adding catalyst and an outlet for discharging heavy component residual liquid, a tower kettle residual liquid outlet of the primary rectification tower 30 and/or a tower kettle residual liquid outlet of the secondary rectification tower 60 are connected with the inlet for introducing rectification residual liquid of the recycling chlorination kettle 80, a condenser 81 for recycling and a condensation receiving groove 82 for recycling are also arranged above the recycling chlorination kettle 80, a tower top gas phase outlet of the recycling chlorination kettle is connected with the condenser 81 for recycling, a first return port of the condenser 81 for recycling is connected with the recycling chlorination kettle 80, a second return port of the condenser 81 for recycling is connected with the condensation receiving groove 82 for recycling, an outlet of the condensation receiving groove 82 for recycling is connected with a recycling semi-finished product groove, the recycling semi-finished product groove is connected with a recycling inlet of the secondary rectification tower 60, a heavy component residual liquid outlet of the recycling chlorination kettle 80 is connected with a hydrolysis kettle 90, the hydrolysis kettle 90 is provided with an inlet for introducing, the entry of adding heavy ends raffinate, the inside rabbling mechanism that sets up of cauldron 90 of hydrolysising, cauldron 90 of hydrolysising still set up the export of discharge raffinate, and cauldron 90 of hydrolysising's exit linkage centrifuge 100, centrifuge 100 sets up fixed residue export and comdenstion water export, and comdenstion water exit linkage comdenstion water buffer tank.
Further, the recycling system comprises a sulfur melting kettle 10, a primary chlorination kettle 20, a primary rectifying tower 30, a semi-finished product kettle 40, a secondary chlorination kettle 50, a secondary rectifying tower 60, a finished product kettle 70, a recycling chlorination kettle 80, a hydrolysis kettle 90, a centrifugal machine 100 and a distillation kettle 200, wherein the sulfur melting kettle 10 is provided with an inlet for introducing chlorine, an inlet for adding sulfur and an outlet for discharging sulfur, the outlet of the sulfur melting kettle 10 is connected with a disulfide dichloride inlet of the primary chlorination kettle 20, the primary chlorination kettle 20 is also provided with an inlet for introducing chlorine, an inlet for introducing chloroacetic acid mother liquor and an outlet for discharging a mixture containing acyl chloride, the outlet of the chlorination kettle is connected with the primary rectifying tower 30 in sequence, the primary rectifying tower 30 is provided with a tower top gas phase outlet, a reflux port and a tower bottom residual liquid outlet, a primary condenser 31 and a primary condensation receiving tank 32 are arranged above the primary rectifying tower 30, the primary condenser 31 is used for refluxing the mixture containing acyl chloride to the primary condensation receiving tank 32, the heavy component residual liquid is refluxed into the primary rectifying tower 30, an outlet of the primary condensation receiving tank 32 is connected with the semi-finished product kettle 40, an outlet of the semi-finished product kettle 40 is connected with an inlet of the secondary chlorination kettle 50, the secondary chlorination kettle 50 is provided with an inlet for introducing chlorine gas, an inlet for adding catalyst and an outlet, an outlet of the secondary chlorination kettle 50 is connected with an inlet of the secondary rectifying tower 60, the secondary rectifying tower 60 is provided with a recovery inlet, a light component outlet at the top of the tower and a residual liquid outlet at the bottom of the tower, and the finished product kettle 70 is connected with the light component substances condensed by the secondary rectifying tower 60; the recycling chlorination kettle 80 is provided with an inlet for introducing chlorine, an inlet for introducing rectification residual liquid, an inlet for adding catalyst and an outlet for discharging heavy component residual liquid, a tower kettle residual liquid outlet of the primary rectification tower 30 and/or a tower kettle residual liquid outlet of the secondary rectification tower 60 are connected with the inlet for introducing rectification residual liquid of the recycling chlorination kettle 80, a condenser 81 for recycling and a condensation receiving groove 82 for recycling are also arranged above the recycling chlorination kettle 80, a tower top gas phase outlet of the recycling chlorination kettle is connected with the condenser 81 for recycling, a first return port of the condenser 81 for recycling is connected with the recycling chlorination kettle 80, a second return port of the condenser 81 for recycling is connected with the condensation receiving groove 82 for recycling, an outlet of the condensation receiving groove 82 for recycling is connected with a recycling semi-finished product groove, the recycling semi-finished product groove is connected with a recycling inlet of the secondary rectification tower 60, a heavy component residual liquid outlet of the recycling chlorination kettle 80 is connected with a hydrolysis kettle 90, the hydrolysis kettle 90 is provided with an inlet for introducing, an inlet for adding heavy component residual liquid, a stirring mechanism is arranged in the hydrolysis kettle 90, the hydrolysis kettle 90 is also provided with an outlet for discharging the residual liquid, the outlet of the hydrolysis kettle 90 is connected with a centrifuge 100, the centrifuge 100 is provided with a fixed residue outlet and a condensed water outlet, and the condensed water outlet is connected with a condensed water buffer tank; the distillation still 200 is provided with an inlet for introducing chloroacetic acid mother liquor and an outlet for discharging dehydrated chloroacetic acid, a distillation condenser 201 and a distillation condensation receiving groove 202 are further arranged above the distillation still 200, the top gas phase outlet of the distillation chlorination still is connected with the distillation condenser 201, the first backflow port of the distillation condenser 201 is connected with the distillation still 200, the second backflow port of the distillation condenser 201 is connected with the distillation condensation receiving groove 202, the outlet of the distillation condensation receiving groove 202 is connected with the inlet of the hydrolysis kettle 90 for introducing absorption water, so that chloroacetic acid wastewater is introduced into the hydrolysis kettle 90, the outlet at the bottom of the distillation still 200 is connected with the primary chlorination kettle 20, and dehydrated chloroacetic acid is introduced into the primary chlorination kettle 20.
The modules or units in the device of the embodiment of the invention can be combined, divided and deleted according to actual needs.
The above disclosure is only illustrative of the preferred embodiments of the present invention, which should not be taken as limiting the scope of the invention, but rather the invention can be embodied in other specific forms without departing from the spirit or essential characteristics thereof. It will be understood by those skilled in the art that all or a portion of the above-described embodiments may be practiced and equivalents thereof may be resorted to as falling within the scope of the invention as claimed. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A method for recycling acid wastewater and rectification residual liquid in the production process of trichloroacetyl chloride is characterized by comprising the following steps:
adding a catalyst into the recovery chlorination kettle;
metering and vacuumizing the rectification residual liquid generated in the production process of trichloroacetyl chloride to a recovery chlorination kettle;
heating the recovered chlorination kettle to a preset temperature, introducing chlorine gas, and reacting acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride;
condensing and collecting light component products of the reaction of the recycling chlorination kettle to a recycling semi-finished product tank, then sending to a trichloroacetyl chloride secondary rectifying tower for refining to obtain a trichloroacetyl chloride product, and sending heavy component residual liquid in the recycling chlorination kettle to a hydrolysis kettle;
and introducing water into the hydrolysis kettle to hydrolyze the heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water.
2. The method for recycling acidic wastewater and rectification residue in the trichloroacetyl chloride production process as claimed in claim 1, characterized by comprising the following steps:
adding a catalyst into the recovery chlorination kettle;
metering and vacuumizing the rectification residual liquid generated in the production process of trichloroacetyl chloride to a recovery chlorination kettle;
heating the recovered chlorination kettle to a preset temperature, introducing chlorine gas, and reacting acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride;
condensing and collecting light component products of the reaction of the recycling chlorination kettle to a recycling semi-finished product tank, then sending to a trichloroacetyl chloride secondary rectifying tower for refining to obtain a trichloroacetyl chloride product, and sending heavy component residual liquid in the recycling chlorination kettle to a hydrolysis kettle;
and introducing water into the hydrolysis kettle to hydrolyze the heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water, wherein in the step, the water introduced into the hydrolysis kettle is the acidic wastewater in the chloroacetic acid mother liquor.
3. The method for recycling acidic wastewater and rectification residue in the trichloroacetyl chloride production process as claimed in claim 2, characterized by comprising the following steps:
and (3) pumping the chloroacetic acid mother liquor into a recovery distillation still for distillation and separation, wherein the separated dehydrated chloroacetic acid mother liquor is used as a trichloroacetyl chloride production raw material, and the separated acidic wastewater is sent into a hydrolysis still for hydrolysis of heavy component residual liquid.
4. The method for recycling acidic wastewater and rectification residue in the trichloroacetyl chloride production process as claimed in claim 1, characterized by comprising the following steps:
introducing chlorine and sulfur into the vulcanizing kettle to produce disulfide dichloride;
introducing dichlorinated disulfide, chlorine and chloroacetic acid mother liquor into a primary chlorination kettle, and preparing an acyl chloride mixture through primary chlorination;
the product after primary chlorination is rectified for the first time, the rectified light component is condensed and collected to a semi-finished product kettle, and the heavy component forms primary rectification residual liquid;
introducing chlorine and a catalyst into the secondary chlorination kettle, and feeding the substances in the semi-finished product kettle into the secondary chlorination kettle for secondary chlorination reaction;
secondarily rectifying the product prepared by secondary chlorination, condensing and collecting the rectified light component to a finished product kettle, and forming secondary rectification residual liquid by the heavy component;
adding a catalyst into the recovery chlorination kettle;
metering and vacuumizing the primary rectification residual liquid and the secondary rectification residual liquid to a recovery chlorination kettle;
heating the recovered chlorination kettle to a preset temperature, introducing chlorine gas, and reacting acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride;
condensing and collecting light component products of the reaction of the recycling chlorination kettle to a recycling semi-finished product tank, sending the light component products to a secondary rectifying tower for secondary rectification to obtain trichloroacetyl chloride products, and sending heavy component residual liquid in the recycling chlorination kettle to a hydrolysis kettle;
and introducing water into the hydrolysis kettle to hydrolyze the heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water.
5. The method for recycling acidic wastewater and rectification residue in the trichloroacetyl chloride production process as claimed in claim 1 or 4, characterized by comprising the following steps:
introducing chlorine and sulfur into the vulcanizing kettle to produce disulfide dichloride;
introducing dichlorinated disulfide, chlorine and chloroacetic acid mother liquor into a primary chlorination kettle, and preparing an acyl chloride mixture through primary chlorination;
the product after primary chlorination is rectified for the first time, the rectified light component is condensed and collected to a semi-finished product kettle, and the heavy component forms primary rectification residual liquid;
introducing chlorine and a catalyst into the secondary chlorination kettle, and feeding the substances in the semi-finished product kettle into the secondary chlorination kettle for secondary chlorination reaction;
secondarily rectifying the product prepared by secondary chlorination, condensing and collecting the rectified light component to a finished product kettle, and forming secondary rectification residual liquid by the heavy component;
adding a catalyst into the recovery chlorination kettle;
metering and vacuumizing the primary rectification residual liquid and the secondary rectification residual liquid to a recovery chlorination kettle;
heating the recovered chlorination kettle to a preset temperature, introducing chlorine gas, and reacting acetyl chloride, monochloroacetyl chloride and dichloroacetyl chloride in the rectification residual liquid to generate trichloroacetyl chloride;
condensing and collecting light component products of the reaction of the recycling chlorination kettle to a recycling semi-finished product tank, sending the light component products to a secondary rectifying tower for secondary rectification to obtain trichloroacetyl chloride products, and sending heavy component residual liquid in the recycling chlorination kettle to a hydrolysis kettle;
and introducing water into the hydrolysis kettle to hydrolyze the heavy component residual liquid, and performing centrifugal separation to obtain solid residues and condensed water, wherein in the step, the water introduced into the hydrolysis kettle is the acidic wastewater in the chloroacetic acid mother liquor.
6. The method for recycling acidic wastewater and rectification residue in the trichloroacetyl chloride production process as claimed in claim 5, characterized by comprising the following steps:
and (2) pumping the chloroacetic acid mother liquor into a recovery distillation still for distillation and separation, sending the separated dehydrated chloroacetic acid mother liquor to a primary chlorination still for use as a trichloroacetyl chloride production raw material, and sending the separated acidic wastewater into a hydrolysis still for hydrolysis of heavy component residual liquid.
7. A system for recycling acid wastewater and rectification residual liquid in the production process of trichloro-acetic chloride is characterized in that: comprises a recycling chlorination kettle, a hydrolysis kettle and a centrifugal machine, wherein the recycling chlorination kettle is provided with an inlet for introducing chlorine, an inlet for introducing rectification residual liquid, an inlet for adding a catalyst and an outlet for discharging heavy component residual liquid, a recycling condenser and a recycling condensation receiving groove are also arranged above the recycling chlorination kettle, a tower top gas phase outlet of the recycling chlorination kettle is connected with the recycling condenser, a first return port of the recycling condenser is connected with the recycling chlorination kettle, a second return port of the recycling condenser is connected with the recycling condensation receiving groove, an outlet of the recycling condensation receiving groove is connected with a recycling semi-finished product groove, a heavy component residual liquid outlet of the recycling chlorination kettle is connected with the hydrolysis kettle, the hydrolysis kettle is provided with an inlet for introducing absorption water, an inlet for adding the heavy component residual liquid is arranged in the hydrolysis kettle, a stirring mechanism is arranged in the hydrolysis kettle, the hydrolysis kettle is also provided with an outlet for discharging the heavy component residual liquid, an outlet of the hydrolysis kettle is connected with the centrifugal, the condensed water outlet is connected with a condensed water buffer tank.
8. The system for recycling acidic wastewater and rectification residue in the trichloroacetyl chloride production process as claimed in claim 7, wherein: the recycle system still includes the stills, the stills sets up the entry that lets in the chloroacetic acid mother liquor, the export of the chloroacetic acid mother liquor of dehydration of discharging, still set up the distillation above the stills and use the condenser, the condensation receives the groove for the distillation, the distillation is with the condenser for the top gas phase exit linkage of chlorination cauldron, the stills is connected with the first backward flow mouth of condenser for the distillation, the distillation is connected with the condensation and is received the groove with the second backward flow mouth of condenser for the distillation, the distillation is received the exit linkage of groove with the condensation and is hydrolyzed the entry that the cauldron is used for letting in absorption water, in order to let in the cauldron of hydrolyzing with chloroacetic acid waste.
9. The system for recycling acidic wastewater and rectification residue in trichloroacetyl chloride production process according to claim 7, which comprises a sulfur melting kettle, a primary chlorination kettle, a primary rectification tower, a semi-finished product kettle, a secondary chlorination kettle, a secondary rectification tower, a finished product kettle, a recycling chlorination kettle, a hydrolysis kettle and a centrifuge, wherein the sulfur melting kettle is provided with an inlet for introducing chlorine gas, an inlet for adding sulfur and an outlet for discharging sulfur, the outlet for the sulfur melting kettle is connected with a disulfide dichloride inlet of the primary chlorination kettle, the primary chlorination kettle is also provided with an inlet for introducing chlorine gas, an inlet for introducing chloroacetic acid mother liquor and an outlet for discharging acyl chloride-containing mixture, the outlet for the primary chlorination kettle is connected with the primary rectification tower, the primary rectification tower is provided with a tower top gas phase outlet, a reflux port and a tower bottom residue outlet, a primary condenser and a primary condensation receiving tank are arranged above the primary rectification tower, the primary condenser is used for refluxing the acyl chloride-containing mixture to the primary condensation receiving tank, the heavy component residual liquid is refluxed into a primary rectifying tower, an outlet of a primary condensation receiving groove is connected with a semi-finished product kettle, an outlet of the semi-finished product kettle is connected with an inlet of a secondary chlorination kettle, the secondary chlorination kettle is provided with an inlet for introducing chlorine gas, an inlet for adding catalyst and an outlet, an outlet of the secondary chlorination kettle is connected with an inlet of the secondary rectifying tower, the secondary rectifying tower is provided with a recycling inlet, a light component outlet at the top of the tower and a residual liquid outlet at the bottom of the tower, and the finished product kettle is connected with a light component substance condensed by the secondary rectifying tower; the recycling chlorination kettle is provided with an inlet for introducing chlorine, an inlet for introducing rectification residual liquid, an inlet for adding catalyst and an outlet for discharging heavy component residual liquid, a tower kettle residual liquid outlet of the primary rectification tower and/or a tower kettle residual liquid outlet of the secondary rectification tower are connected with the inlet for introducing rectification residual liquid of the recycling chlorination kettle, a condenser for recycling and a condensation receiving groove for recycling are also arranged above the recycling chlorination kettle, a tower top gas phase outlet of the chlorination kettle for recycling is connected with the condenser for recycling, a first return port of the condenser for recycling is connected with the recycling chlorination kettle, a second return port of the condenser for recycling is connected with the condensation receiving groove for recycling, an outlet of the condensation receiving groove for recycling is connected with a semi-finished product recycling groove, the semi-finished product recycling groove is connected with the recycling inlet of the secondary rectification tower, a heavy component outlet of the recycling chlorination kettle is connected with a hydrolysis kettle, the hydrolysis kettle is provided with an inlet for introducing absorption water, and an inlet for adding heavy, the inside rabbling mechanism that sets up of cauldron of hydrolysising, the cauldron of hydrolysising still set up the export of discharge raffinate, the exit linkage centrifuge of cauldron of hydrolysising, centrifuge set up fixed residue export and comdenstion water export, comdenstion water exit linkage comdenstion water buffer tank.
10. The system for recycling acidic wastewater and rectification residue in the trichloroacetyl chloride production process as claimed in claim 9, wherein: comprises a sulfur melting kettle, a primary chlorination kettle, a primary rectifying tower, a semi-finished product kettle, a secondary chlorination kettle, a secondary rectifying tower, a finished product kettle, a recycling chlorination kettle, a hydrolysis kettle, a centrifugal machine and a distillation kettle, wherein the sulfur melting kettle is provided with an inlet for introducing chlorine, an inlet for adding sulfur and a discharge port, the discharge port of the sulfur melting kettle is connected with a dichlorinated disulfide inlet of the primary chlorination kettle, the primary chlorination kettle is also provided with an inlet for introducing chlorine, an inlet for introducing chloroacetic acid mother liquor and an outlet for discharging acyl chloride-containing mixture, the outlet of the primary chlorination kettle is connected with the primary rectifying tower, the primary rectifying tower is provided with a tower top gas phase outlet, a reflux port and a tower kettle residual liquid outlet, a primary condenser and a primary condensation receiving groove are also arranged above the primary rectifying tower, the primary condenser is used for refluxing the acyl chloride-containing mixture to the primary condensation receiving groove, and is also used for refluxing heavy component residual liquid to the primary rectifying tower, the outlet of the primary, the outlet of the semi-finished product kettle is connected with the inlet of a secondary chlorination kettle, the secondary chlorination kettle is provided with an inlet for introducing chlorine, an inlet for adding a catalyst and an outlet, the outlet of the secondary chlorination kettle is connected with the inlet of a secondary rectifying tower, the secondary rectifying tower is provided with a recovery inlet, a tower top light component outlet and a tower kettle residual liquid outlet, and the finished product kettle is connected with a light component substance condensed by the secondary rectifying tower; the recycling chlorination kettle is provided with an inlet for introducing chlorine, an inlet for introducing rectification residual liquid, an inlet for adding catalyst and an outlet for discharging heavy component residual liquid, a tower kettle residual liquid outlet of the primary rectification tower and/or a tower kettle residual liquid outlet of the secondary rectification tower are connected with the inlet for introducing rectification residual liquid of the recycling chlorination kettle, a condenser for recycling and a condensation receiving groove for recycling are also arranged above the recycling chlorination kettle, a tower top gas phase outlet of the chlorination kettle for recycling is connected with the condenser for recycling, a first return port of the condenser for recycling is connected with the recycling chlorination kettle, a second return port of the condenser for recycling is connected with the condensation receiving groove for recycling, an outlet of the condensation receiving groove for recycling is connected with a semi-finished product recycling groove, the semi-finished product recycling groove is connected with the recycling inlet of the secondary rectification tower, a heavy component outlet of the recycling chlorination kettle is connected with a hydrolysis kettle, the hydrolysis kettle is provided with an inlet for introducing absorption water, and an inlet for adding heavy, the inside of the hydrolysis kettle is provided with a stirring mechanism, the hydrolysis kettle is also provided with an outlet for discharging residual liquid, the outlet of the hydrolysis kettle is connected with a centrifuge, the centrifuge is provided with a fixed residue outlet and a condensed water outlet, and the condensed water outlet is connected with a condensed water buffer tank; the stills sets up the entry that lets in the chloroacetic acid mother liquor, the export of the dehydration chloroacetic acid of discharging, still set up the distillation in the stills top and use the condenser, the distillation receives the groove with the condensation, the distillation is with the overhead gaseous phase exit linkage of chlorination cauldron condenser for the distillation, the still is connected with the first backward flow mouth of condenser for the distillation, the distillation is with the second backward flow mouth of condenser connection distillation and is received the groove with the condensation, the distillation receives the entry that the exit linkage hydrolysis cauldron in groove is used for letting in absorption water with the condensation, in order to let in the hydrolysis cauldron with chloroacetic acid waste water, chlorination cauldron is once carried out to stills bottom exit linkage, in order to let in chlorination cauldron once with dehydration chloroacetic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110018989.9A CN112830875A (en) | 2021-01-07 | 2021-01-07 | Method and system for recycling acid wastewater and rectification residual liquid in trichloro-acetic chloride production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110018989.9A CN112830875A (en) | 2021-01-07 | 2021-01-07 | Method and system for recycling acid wastewater and rectification residual liquid in trichloro-acetic chloride production process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112830875A true CN112830875A (en) | 2021-05-25 |
Family
ID=75927901
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110018989.9A Pending CN112830875A (en) | 2021-01-07 | 2021-01-07 | Method and system for recycling acid wastewater and rectification residual liquid in trichloro-acetic chloride production process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112830875A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114835575A (en) * | 2022-05-27 | 2022-08-02 | 成武县晨晖环保科技有限公司 | Method for producing chloroacetic acid mixed acid and trichloro-acetyl chloride by using residues in chloroacetyl chloride production process |
| CN117819782A (en) * | 2024-03-05 | 2024-04-05 | 河南嘉颖生物科技有限公司 | Comprehensive utilization process and device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086870A (en) * | 2011-10-27 | 2013-05-08 | 山西三维丰海化工有限公司 | Novel process for producing trichloro-acetic chloride |
| CN103709028A (en) * | 2013-12-09 | 2014-04-09 | 江苏省格林艾普化工股份有限公司 | Distillation recovery method of chloroacetic acid mother liquor |
| CN106748739A (en) * | 2015-11-20 | 2017-05-31 | 宁夏际华环境安全科技有限公司 | A kind of trichloro-acetic chloride production technology |
| CN112409164A (en) * | 2021-01-19 | 2021-02-26 | 潍坊滨海石油化工有限公司 | Treatment method of mother liquor produced by chloroacetic acid preparation through hydrogenation method |
-
2021
- 2021-01-07 CN CN202110018989.9A patent/CN112830875A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086870A (en) * | 2011-10-27 | 2013-05-08 | 山西三维丰海化工有限公司 | Novel process for producing trichloro-acetic chloride |
| CN103709028A (en) * | 2013-12-09 | 2014-04-09 | 江苏省格林艾普化工股份有限公司 | Distillation recovery method of chloroacetic acid mother liquor |
| CN106748739A (en) * | 2015-11-20 | 2017-05-31 | 宁夏际华环境安全科技有限公司 | A kind of trichloro-acetic chloride production technology |
| CN112409164A (en) * | 2021-01-19 | 2021-02-26 | 潍坊滨海石油化工有限公司 | Treatment method of mother liquor produced by chloroacetic acid preparation through hydrogenation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114835575A (en) * | 2022-05-27 | 2022-08-02 | 成武县晨晖环保科技有限公司 | Method for producing chloroacetic acid mixed acid and trichloro-acetyl chloride by using residues in chloroacetyl chloride production process |
| CN117819782A (en) * | 2024-03-05 | 2024-04-05 | 河南嘉颖生物科技有限公司 | Comprehensive utilization process and device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid |
| CN117819782B (en) * | 2024-03-05 | 2024-05-10 | 河南嘉颖生物科技有限公司 | Comprehensive utilization process and device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112830875A (en) | Method and system for recycling acid wastewater and rectification residual liquid in trichloro-acetic chloride production process | |
| CN102417162B (en) | Recycling method of hydrochloric acid-acetic acid waste liquid | |
| CN101560151A (en) | Process for continuously generating methyl acetate by reactive distillation taking ionic liquid as catalyst | |
| CN110922292B (en) | Preparation method of chloromethane | |
| CN114852960A (en) | Method and device for two-phase separation, concentration and purification in sulfur-iodine circulation hydrogen production | |
| CN102030627B (en) | Process for recovering valued compounds from a stream derived from purification of methyl methacrylate | |
| CN104761452A (en) | Purification method for butyl acrylate crude product | |
| CN112724047B (en) | Device and method for preparing trifluoro methanesulfonyl fluoride | |
| EP0460110B1 (en) | Process for the continuous recovery of hydrogen fluoride gas | |
| CN115746048A (en) | Full continuous flow production method of tris (1-chloro-2-propyl) phosphate | |
| CN111072480A (en) | Method for producing methyl ethyl carbonate by using ionic liquid catalysis ester exchange method | |
| CN108689799B (en) | Green synthesis method of chlorocyclohexane | |
| CN113402381A (en) | Preparation method of chloroacetyl chloride | |
| EP4058411A1 (en) | A process for working up water containing 4,4'-dichlorodiphenyl sulfoxide and/or 4,4'-dichlorodiphenyl sulfone as impurities | |
| CN217265503U (en) | Pentafluorophenol's synthesis system | |
| CN111039780A (en) | Process for producing aramid polymerized monomer by thionyl chloride method | |
| CN112973594B (en) | Trans-1, 2-dichloroethylene preparation system for crude product alkaline washing absorption | |
| JP3866876B2 (en) | Method for recovering dimethyl terephthalate | |
| CN116082151A (en) | Synthesis method of S-2-methyl chloropropionate | |
| CN108821254B (en) | Method for removing inorganic and organic impurities in phosphorus trichloride synthesis process | |
| CN1420116A (en) | Process and apparatus for synthesis of thiophene | |
| CA1121829A (en) | Continuous manufacture of allyl diglycol carbonate | |
| CN211863950U (en) | Vinylpyridine compound industrialization device that divides water | |
| CN106800299A (en) | The quick preparation technology of high-purity boron trifluoride and recovery process for purification | |
| CN115724819B (en) | Device for preparing ethylene carbonate and preparation method of ethylene carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210525 |
|
| RJ01 | Rejection of invention patent application after publication |