CN105906485A - Device and process for producing high-purity parachlorophenol - Google Patents
Device and process for producing high-purity parachlorophenol Download PDFInfo
- Publication number
- CN105906485A CN105906485A CN201610283604.0A CN201610283604A CN105906485A CN 105906485 A CN105906485 A CN 105906485A CN 201610283604 A CN201610283604 A CN 201610283604A CN 105906485 A CN105906485 A CN 105906485A
- Authority
- CN
- China
- Prior art keywords
- parachlorophenol
- purity
- reactor
- phenol
- chlorine
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/01—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis
- C07C37/02—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis by substitution of halogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09D161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C09D161/14—Modified phenol-aldehyde condensates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- 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
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a device and a process for producing high-purity parachlorophenol. The device comprises a reaction kettle, a storage tank, a distillation tower, a collecting tank, a condensation tank, a pressure reducing tower, a separator and a product tank. The device and the process have the advantages that the high-purity parachlorophenol can be produced by the aid of the device and is high in yield; reaction causes little pollution; a gas flow meter is arranged on a chlorine flowing pipeline of the device, accordingly, the inlet quantity of gas can be effectively controlled, and deep reaction can be prevented; a temperature measuring opening is formed in the top of a reactor and can bring convenience for measuring the temperatures, and accordingly side reaction due to excessively high temperatures and influence on the purity and the quality of products can be prevented.
Description
Technical field
The present invention relates to chemical technology field, particularly relate to process units and the production technology thereof of a kind of high-purity parachlorophenol.
Background technology
Parachlorophenol is a kind of for system dye and medicine, also serves as the denaturant of ethanol and the selective solvent etc. of refined mineral oil.Can be additionally used in microscopic analysis, pharmaceuticals industry, plant growth promoter, it is possible to apply in the middle of medicine, pesticide and the every field such as dyestuff and other organic synthesis raw materials, be of wide application.In prior art, the production of parachlorophenol can be mixed a lot of impurity, it is impossible to extract highly purified parachlorophenol, and discharged a lot of waste gas during extracting parachlorophenol simultaneously, cause environmental pollution.
Summary of the invention
The technical problem to be solved is to provide process units and the production technology thereof of a kind of high-purity parachlorophenol, not only increases the purity of transformation efficiency and parachlorophenol, and decreases environmental pollution.
nullFor achieving the above object,The present invention provides following technical scheme: disclose the process units of a kind of high-purity parachlorophenol,Including reactor (1)、Storage tank (2)、Distillation column (3)、Rewinding tank (4)、Drainer (5)、Vacuum tower (6),Separator (7)、Products pot (8),Described reactor (1) top is provided with charging aperture,It is provided with discharging opening bottom described reactor,It is provided with between described reactor (1) with storage tank (2) and is connected pipeline and the first centrifugal pump (12),It is provided with between discharging opening and the described distillation column (3) of described reactor (1) bottom and is connected pipeline and the second centrifugal pump (13),It is provided with between described rewinding tank (4) and distillation column (3) tower top and is connected pipeline,Described drainer (5) is provided with and is connected pipeline and the 3rd centrifugal pump (14) between at the bottom of distillation column (3) tower,It is provided with between described vacuum tower (6) with described drainer (5) and is connected pipeline and the 4th centrifugal pump (15),It is provided with between described vacuum tower (6) with described separator (7) and is connected pipeline and the 5th centrifugal pump (16),It is provided with between described separator (7) with described products pot (8) and is connected pipeline and the 6th centrifugal pump (17);
Being additionally provided with corrosion-inhibiting coating on described reactor (1) inwall, described corrosion-inhibiting coating is formed on reactor (1) inwall by anti-corrosion paint, and described anticorrosive paint is mixed by first and second liang of components, counts first in mass ratio: second=11:4;
Described first component includes following components according to the mass fraction: Firebrake ZB phenol-formaldehyde resin modified: 25-31 part, sodium carboxymethyl cellulose: 11-14 part, filler: 8-14 part, silica flour: 6-14 part, dispersant: 3-7 part, coalescents: 2-5 part, organosilicon: 3
-8 parts;
Described second component includes following components according to the mass fraction: polyphenylene oxide resin powder: 28-30 part, xylene formaldehyde resin: 2-7 part, isopropanol 3-6 part, toluene: 8-11 part, plasticizer: 5-8 part, alkylolamides polyethylene oxide ether: 1-3 part, coupling agent: 8-10 part;
Wherein, described filler glass flake or aluminium oxide one therein, described dispersant is the one in sodium tetrapolyphosphate or sodium hexameta phosphate, and described coalescents is the one in ethylene glycol, ethylene glycol or propylene glycol;
Described plasticizer is the one in dioctyl phthalate or dibutyl phthalate, and described coupling agent is at least one in silane coupler or zirconium class coupling agent.
The present invention limits technical scheme, the process units of aforesaid high-purity parachlorophenol further, and described reactor (1) bottom is provided with chlorine pipeline.
The process units of aforesaid high-purity parachlorophenol, described chlorine pipeline is provided with gas flowmeter (10).
The process units of aforesaid high-purity parachlorophenol, described reactor (1) top is provided with temperature survey mouth (9).
The process units of aforesaid high-purity parachlorophenol, reactor (1) bottom is provided with air bleeding valve (11).
The process units of aforesaid high-purity parachlorophenol, it is characterised in that described connection pipeline is all DN40 corrosion-proof steel pipe;Composition and the mass percent of the steel of described connection pipeline be: C:0.45-0.49%, Si:0.18-0.21%, Ti:0.66-0.79%, Al:0.53-0.57%, Cu:0.09-0.15%, Mn:0.66-0.68%, Ni:0.83-0.85%, Cr:4.1-6.3%, Mo:0.55-0.57%, V:0.13-0.15%, Nb:0.11-0.13%, and lanthanide rare: 0.35-0.43%, surplus are Fe and inevitable impurity;The constituent mass percentage ratio of described lanthanide rare is: cerium: 2-4%, neodymium: 11-13%, gadolinium: 3-5%, lutecium: 4-6%, dysprosium: 5-7%, praseodymium: 12-15%, holmium: 0-4%, erbium: 15-20%, and surplus is lanthanum, and above each component sum is 100%.
A kind of production technology of high-purity parachlorophenol, described production craft step is as follows:
(1) phenol in storage tank is squeezed in phenol preheater by conveying pipe, open steam valve and phenol is heated generation liquid;
(2) phenol generating liquid flows in reactor, add solvent and catalyst, then 20-25min is stirred, and it is gradually heated to 66-70 DEG C, open chlorine ingress pipe valve in reactor, be passed through chlorine, controlling into chlorine speed is that 15g/h-28g/h makes chlorine add in 3-5h, keeps the temperature within reactor to be 75-85 DEG C, continues stirring 15-20min and obtains mixed phenol.
Wherein, described phenol based on the amount ratio of material: chlorine: catalyst=1:1.6-1.8:0.005;
(3) mixed phenol gradually heats up after entering steam tank, and intensification rear-guard rushes to crude product tank and then carries out rectification, stops rectification after rectification temperature 80-85 DEG C;
(4) flow into filtration in crystallizer after the rectification debris in step (3) is down to room temperature, i.e. can get high-purity parachlorophenol crystal after drying.
Employing technical scheme provides the benefit that: assembly of the invention can produce highly purified parachlorophenol, and yield is high, the produced pollution is the most fewer in the reaction, this device is provided with gas flowmeter on the pipeline of logical chlorine, it is possible to the effective air inflow controlling gas, it is to avoid deep reaction, it is provided with temperature survey mouth in reactor head, it is easy to temperature detection, the side reaction preventing too high temperature from being brought, affect purity and the quality of product.The reactor corrosion-inhibiting coating suitability of present invention design is strong, pollutes little and low cost, and has stronger humidity and corrosion resistance, reactor can be made unaffected in the case of being used for multiple times;Use the anti-corrosion pipeline of special steel grade, add the service life of pipeline, decrease the risk of equipment leakage, reduce cost of equipment maintenance;And the production technology of parachlorophenol is simple, uses phenol as raw material, reduces production cost, protect environment, improve work efficiency in technique.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention;
1-reactor, 2-storage tank, 3-distillation column, 4-rewinding tank, 5-drainer, 6-vacuum tower, 7-separator, 8-products pot, 9-temperature survey mouth, 10-gas flowmeter, 11-air bleeding valve, 12-the first centrifugal pump, 13-the second centrifugal pump, 14-the 3rd centrifugal pump, 15-the 4th centrifugal pump, 16-the 5th centrifugal pump, 17-the 6th centrifugal pump.
Detailed description of the invention
Embodiment 1
The present embodiment provides the process units of a kind of high-purity parachlorophenol, and structure is as it is shown in figure 1, include reactor 1, storage tank 2, distillation column 3, rewinding tank 4, drainer 5, vacuum tower 6, separator 7, products pot 8;Reactor top is provided with charging aperture and temperature survey mouth 9, discharging opening it is provided with bottom reactor, chlorine pipeline and air bleeding valve, chlorine pipeline is provided with gas flowmeter 10, it is provided with between reactor 1 with storage tank 2 and is connected pipeline and the first centrifugal pump 12, discharging opening bottom reactor 1 is connected pipeline and the second centrifugal pump 13 with being provided with between distillation column 3, it is provided with between rewinding tank 4 with distillation column 3 tower top and is connected pipeline, drainer 5 is provided with and is connected pipeline and the 3rd centrifugal pump 14 between at the bottom of distillation column 4 tower, it is provided with between vacuum tower 6 with drainer 5 and is connected pipeline and the 4th centrifugal pump 15, it is provided with between vacuum tower 6 with separator 7 and is connected pipeline and the 5th centrifugal pump 16, it is provided with between separator 7 with products pot 8 and is connected pipeline and the 6th centrifugal pump 17, all of pipeline all uses DN40 corrosion-proof steel pipe;The composition of steel and the mass percent that connect pipeline be: C:0.47%, Si:0.19%, Ti:0.69%, Al:0.55%, Cu:0.
15%, Mn:0.
68%, Ni:0.83%, Cr:4.3%, Mo:0.55%, V:0.15%, Nb:0.13%, lanthanide rare: 0.43%, surplus is Fe and inevitable impurity;The constituent mass percentage ratio of lanthanide rare is: cerium: 4%, neodymium: 11%, gadolinium: 3%, lutecium: 6%, dysprosium: 5%, praseodymium: 14%, holmium: 2%, erbium: 18%, and surplus is lanthanum, and above each component sum is 100%.
Phenol is sent in reactor by this device by the first centrifugal pump, it is stirred by agitator, a certain amount of benzene is added when phenol is in melted, continue stirring, it is passed through chlorine to react, when the temperature of chlorated liquid is at about 25 DEG C, open the air bleeding valve bottom reactor, get rid of the hydrogen chloride gas produced in reaction, then distillation column is sent to distill material, benzene distills out from distillation column top to be delivered to rewinding tank, remaining material is sent into drainer by the 3rd centrifugal pump and is condensed, when temperature is to 80 DEG C, it is sent to vacuum tower by the 4th centrifugal pump, it is re-fed into separator to separate, parachlorophenol is separated and is sent to products pot.
Being additionally provided with corrosion-inhibiting coating on the reactor inwall of the present embodiment, corrosion-inhibiting coating is formed on reactor inwall by anti-corrosion paint, and anticorrosive paint is mixed by first and second liang of components, counts first in mass ratio: second=11:4;
First component includes following components according to the mass fraction: Firebrake ZB phenol-formaldehyde resin modified: 27 parts, sodium carboxymethyl cellulose: 13 parts, glass flake: 11 parts, silica flour: 8 parts, sodium tetrapolyphosphate: 4 parts, ethylene glycol: 4 parts, organosilicon: 3 parts;
Described second component includes following components according to the mass fraction: polyphenylene oxide resin powder: 28 parts, xylene formaldehyde resin: 5 parts, isopropanol: 3 parts, toluene: 11 parts, dibutyl phthalate: 6 parts, alkylolamides polyethylene oxide ether: 2 parts, silane coupler: 10 parts.
The production craft step of high-purity parachlorophenol is as follows:
(1) phenol in storage tank is squeezed in phenol preheater by conveying pipe, open steam valve and phenol is heated generation liquid;
(2) phenol generating liquid flows in reactor, add solvent and catalyst, then 23min is stirred, and it is gradually heated to 38 DEG C, open chlorine ingress pipe valve in reactor, be passed through chlorine, controlling into chlorine speed is that 22g/h makes chlorine add in 4h, and keeping the temperature within reactor is 80 DEG C, continues stirring 15min and obtains mixed phenol;
Wherein, described phenol based on the amount ratio of material: chlorine: catalyst=1:1.6:0.005;
(3) mixed phenol gradually heats up after entering steam tank, and intensification rear-guard rushes to crude product tank and then carries out rectification, stops rectification after rectification temperature 82 DEG C;
(4) flow into filtration in crystallizer after the rectification debris in step (3) is down to room temperature, i.e. can get high-purity parachlorophenol crystal after drying.
In addition to the implementation, the present invention can also have other embodiments.The technical scheme that all employing equivalents or equivalent transformation are formed, all falls within the protection domain of application claims.
Claims (8)
- null1. the process units of a high-purity parachlorophenol,Including reactor (1)、Storage tank (2)、Distillation column (3)、Rewinding tank (4)、Drainer (5)、Vacuum tower (6),Separator (7)、Products pot (8),It is characterized in that: described reactor (1) top is provided with charging aperture,It is provided with discharging opening bottom described reactor,It is provided with between described reactor (1) with storage tank (2) and is connected pipeline and the first centrifugal pump (12),It is provided with between discharging opening and the described distillation column (3) of described reactor (1) bottom and is connected pipeline and the second centrifugal pump (13),It is provided with between described rewinding tank (4) and distillation column (3) tower top and is connected pipeline,Described drainer (5) is provided with and is connected pipeline and the 3rd centrifugal pump (14) between at the bottom of distillation column (3) tower,It is provided with between described vacuum tower (6) with described drainer (5) and is connected pipeline and the 4th centrifugal pump (15),It is provided with between described vacuum tower (6) with described separator (7) and is connected pipeline and the 5th centrifugal pump (16),It is provided with between described separator (7) with described products pot (8) and is connected pipeline and the 6th centrifugal pump (17);Being additionally provided with corrosion-inhibiting coating on described reactor (1) inwall, described corrosion-inhibiting coating is formed on reactor (1) inwall by anti-corrosion paint, and described anticorrosive paint is mixed by first and second liang of components, counts first in mass ratio: second=11:4;Described first component includes following components according to the mass fraction: Firebrake ZB phenol-formaldehyde resin modified: 25-31 part, sodium carboxymethyl cellulose: 11-14 part, filler: 8-14 part, silica flour: 6-14 part, dispersant: 3-7 part, coalescents: 2-5 part, organosilicon: 3-8 parts;Described second component includes following components according to the mass fraction: polyphenylene oxide resin powder: 28-30 part, xylene formaldehyde resin: 2-7 part, isopropanol 3-6 part, toluene: 8-11 part, plasticizer: 5-8 part, alkylolamides polyethylene oxide ether: 1-3 part, coupling agent: 8-10 part;Wherein, described filler glass flake or aluminium oxide one therein, described dispersant is the one in sodium tetrapolyphosphate or sodium hexameta phosphate, and described coalescents is the one in ethylene glycol, ethylene glycol or propylene glycol;Described plasticizer is the one in dioctyl phthalate or dibutyl phthalate, and described coupling agent is at least one in silane coupler or zirconium class coupling agent.
- The process units of high-purity parachlorophenol the most according to claim 1, it is characterised in that described reactor (1) bottom is provided with chlorine pipeline.
- The process units of high-purity parachlorophenol the most according to claim 2, it is characterised in that described chlorine pipeline is provided with gas flowmeter (10).
- The process units of high-purity parachlorophenol the most according to claim 1, it is characterised in that described reactor (1) top is provided with temperature survey mouth (9).
- The process units of high-purity parachlorophenol the most according to claim 4, it is characterised in that described reactor (1) bottom is provided with air bleeding valve (11).
- The process units of high-purity parachlorophenol the most according to claim 1, it is characterised in that described connection pipeline is all DN40 corrosion-proof steel pipe.
- The process units of high-purity parachlorophenol the most according to claim 6, it is characterized in that, composition and the mass percent of the steel of described connection pipeline be: C:0.45-0.49%, Si:0.18-0.21%, Ti:0.66-0.79%, Al:0.53-0.57%, Cu:0.09-0.15%, Mn:0.66-0.68%, Ni:0.83-0.85%, Cr:4.1-6.3%, Mo:0.55-0.57%, V:0.13-0.15%, Nb:0.11-0.13%, and lanthanide rare: 0.35-0.43%, surplus are Fe and inevitable impurity;The constituent mass percentage ratio of described lanthanide rare is: cerium: 2-4%, neodymium: 11-13%, gadolinium: 3-5%, lutecium: 4-6%, dysprosium: 5-7%, praseodymium: 12-15%, holmium: 0-4%, erbium: 15-20%, and surplus is lanthanum, and above each component sum is 100%.
- 8. according to the process units of the high-purity parachlorophenol described in any claim in 1-6, it is characterised in that also including the production technology of a kind of high-purity parachlorophenol, described production craft step is as follows:(1) phenol in storage tank is squeezed in phenol preheater by conveying pipe, open steam valve and phenol is heated generation liquid;(2) phenol generating liquid flows in reactor, add solvent and catalyst, then 20-25min is stirred, and it is gradually heated to 66-70 DEG C, open chlorine ingress pipe valve in reactor, be passed through chlorine, controlling into chlorine speed is that 15g/h-28g/h makes chlorine add in 3-5h, keeps the temperature within reactor to be 75-85 DEG C, continues stirring 15-20min and obtains mixed phenol;Wherein, described phenol based on the amount ratio of material: chlorine: catalyst=1:1.6-1.8:0.005;(3) mixed phenol gradually heats up after entering steam tank, and intensification rear-guard rushes to crude product tank and then carries out rectification, stops rectification after rectification temperature 80-85 DEG C;(4) flow into filtration in crystallizer after the rectification debris in step (3) is down to room temperature, i.e. can get high-purity parachlorophenol crystal after drying.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610283604.0A CN105906485A (en) | 2016-05-03 | 2016-05-03 | Device and process for producing high-purity parachlorophenol |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610283604.0A CN105906485A (en) | 2016-05-03 | 2016-05-03 | Device and process for producing high-purity parachlorophenol |
Publications (1)
Publication Number | Publication Date |
---|---|
CN105906485A true CN105906485A (en) | 2016-08-31 |
Family
ID=56753400
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610283604.0A Pending CN105906485A (en) | 2016-05-03 | 2016-05-03 | Device and process for producing high-purity parachlorophenol |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN105906485A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108101750A (en) * | 2018-01-24 | 2018-06-01 | 淮海工学院 | A kind of high-purity parachlorophenol preparation process |
CN116272675A (en) * | 2023-02-20 | 2023-06-23 | 安徽瑞柏新材料有限公司 | Propyl acetate preparation facilities based on catalytic distillation method |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104231857A (en) * | 2014-09-18 | 2014-12-24 | 江苏海晟涂料有限公司 | Composite epoxy anticorrosive paint and preparation method thereof |
CN105257942A (en) * | 2015-11-10 | 2016-01-20 | 江苏宇恒电气有限公司 | Wear and corrosion resistance type bellow expansion joint |
CN105331901A (en) * | 2015-11-27 | 2016-02-17 | 无锡市华尔泰机械制造有限公司 | S22253 duplex stainless steel material flange and production process thereof |
-
2016
- 2016-05-03 CN CN201610283604.0A patent/CN105906485A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104231857A (en) * | 2014-09-18 | 2014-12-24 | 江苏海晟涂料有限公司 | Composite epoxy anticorrosive paint and preparation method thereof |
CN105257942A (en) * | 2015-11-10 | 2016-01-20 | 江苏宇恒电气有限公司 | Wear and corrosion resistance type bellow expansion joint |
CN105331901A (en) * | 2015-11-27 | 2016-02-17 | 无锡市华尔泰机械制造有限公司 | S22253 duplex stainless steel material flange and production process thereof |
Non-Patent Citations (1)
Title |
---|
东北制药总厂中心试验室: "苯酚氯化合成邻位及对位氯苯酚中试", 《辽宁化工》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108101750A (en) * | 2018-01-24 | 2018-06-01 | 淮海工学院 | A kind of high-purity parachlorophenol preparation process |
CN116272675A (en) * | 2023-02-20 | 2023-06-23 | 安徽瑞柏新材料有限公司 | Propyl acetate preparation facilities based on catalytic distillation method |
CN116272675B (en) * | 2023-02-20 | 2023-10-17 | 安徽瑞柏新材料有限公司 | Propyl acetate preparation facilities based on catalytic distillation method |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102977667B (en) | Metal antirust paint containing modified water-soluble nanometer silica sol, and its preparation method | |
CN103205181B (en) | A kind of nanometer heavy-duty coating | |
CN105906485A (en) | Device and process for producing high-purity parachlorophenol | |
CN109370364A (en) | It is a kind of for relating to the nano anticorrosive coating and preparation method thereof of metal surface under acid environment | |
CN104650785B (en) | A kind of boron modified phenolic resin sizing agent | |
CN104774527A (en) | Preparation method of epoxy glass flake coating for oceanic tidal range/splash zone | |
CN202778451U (en) | Apparatus for chloroacetic acid making | |
CN103214655B (en) | Modified epoxy resin and high-solid anticorrosive coating prepared therewith | |
CN104592916B (en) | A kind of making method of boron modified phenolic resin sizing agent | |
CN204582594U (en) | A kind of spent organic solvent regeneration purifying plant | |
CN102977768B (en) | Metal antirust paint prepared from modified phenolic resin, and its preparation method | |
CN102382548A (en) | Solvent-free epoxy coating for inner wall of petroleum storage tank and preparation method | |
CN206739942U (en) | A kind of anticorrosive paint production composite condensator | |
CN104672398A (en) | Efficient production system for unsaturated resin | |
CN108359296A (en) | A kind of inner and outer walls of pipeline anti-corrosion material and preparation method thereof | |
CN105884583A (en) | High-purity 2, 4, 6- trichlorophenol production device and production process thereof | |
CN109180461A (en) | A kind of method that micro-reacting tcchnology prepares butyric acid | |
CN105820673A (en) | Acid-resistant, hydrogen-sulfide-resistant and wear-resistant flexible corrosion prevention coating and preparation method thereof | |
CN204550445U (en) | A kind of High-efficient Production system for unsaturated polyester | |
CN107353743A (en) | A kind of anticorrosion S bend pipe road | |
CN104710938A (en) | Vinyl glass flake coating applied to high temperature resistant strong acid occasions and preparation method thereof | |
CN105906483A (en) | Production device and production process of high-purity o-chlorphenol | |
CN201981139U (en) | Novel pure benzene producing device | |
CN205613388U (en) | Negative pressure condensation reaction system | |
CN205479572U (en) | Safety -valve that corrosion resistance is strong |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160831 |
|
RJ01 | Rejection of invention patent application after publication |