CN105906483A - Production device and production process of high-purity o-chlorphenol - Google Patents
Production device and production process of high-purity o-chlorphenol Download PDFInfo
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- CN105906483A CN105906483A CN201610296699.XA CN201610296699A CN105906483A CN 105906483 A CN105906483 A CN 105906483A CN 201610296699 A CN201610296699 A CN 201610296699A CN 105906483 A CN105906483 A CN 105906483A
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- 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
- C07C37/62—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by introduction of halogen; by substitution of halogen atoms by other halogen atoms
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- 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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- 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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C39/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring
- C07C39/24—Halogenated derivatives
- C07C39/26—Halogenated derivatives monocyclic monohydroxylic containing halogen bound to ring carbon atoms
- C07C39/27—Halogenated derivatives monocyclic monohydroxylic containing halogen bound to ring carbon atoms all halogen atoms being bound to ring carbon atoms
- C07C39/28—Halogenated derivatives monocyclic monohydroxylic containing halogen bound to ring carbon atoms all halogen atoms being bound to ring carbon atoms the halogen being one chlorine atom
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Abstract
The invention discloses a production device and production process of high-purity o-chlorphenol. The production process comprises the following steps of (1) injecting phenol in a material storage tank into a phenol preheating device through a conveying pipe; opening a steam valve and heating the phenol to generate liquid-stage phenol; (2) flowing the generated liquid-state phenol into a reaction kettle; adding 2-irgasan, solvents and catalysts, then, stirring the materials for 20 to 25 min, gradually heating the materials to 66 to 70 DEG C, opening a chlorine gas introduction pipe valve to introduce chlorine gas into the reaction kettle, controlling the chlorine gas introducing speed at 15g/h to 28g/h so that the introduction of the chlorine gas is completed in 3 to 5h, maintaining the temperature inside the reaction kettle to be 150 DEG C to 160 DEG C; continuously stirring the materials for 15 to 20 min to obtain mixed phenol; (3) feeding the mixed phenol into a steam tank, then gradually raising the temperature, driving the materials into a coarse product tank, sequentially performing rectification, and stopping the rectification when the rectification temperature reaches 175 to 180 DEG C; (4) lowering the temperature of the rectification residue liquid in the step (3) to the room temperature, flowing the residue liquid into a crystallizer, performing filtering and drying, and obtaining high-purity o-chlorphenol crystals. The production device and the production process have the advantages that the purity of the o-chlorphenol is improved; the environment pollution is reduced.
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 o chlorophenol.
Background technology
O-chlorphenol is a kind of colourless liquid having abnormal flavour, is slightly soluble in water, also is soluble in the organic solvent such as ethanol, ether, o-chlorphenol is inflammable, can produce the harmful gas such as carbon monoxide, hydrogen chloride, the most toxic (low toxicity), can be through skin absorption, in prior art, a lot of impurity can be mixed, it is impossible to extract highly purified o-chlorphenol in the production of o-chlorphenol, and, during extracting o-chlorphenol, discharge a lot of waste gas 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 o chlorophenol, not only increases the purity of work efficiency and o-chlorphenol, and decreases environmental pollution.
nullFor achieving the above object，The present invention provides following technical scheme: the process units of a kind of high-purity o chlorophenol，Including storage tank、Reaction unit、Exhaust gas absorption device、Fractionating device and purifying plant，Storage tank is connected with reaction unit，Reaction unit includes phenol preheater、Reactor、Chlorine ingress pipe、Thermometer、Steam tank and crude product tank，The side of storage tank bottom is connected with the charging aperture of phenol preheater by conveying pipe，The discharging opening of phenol preheater is connected with the charging aperture of reactor by conveying pipe，The side of reactor upper end is provided with thermometer，The inside of reactor is located in one end of thermometer，The opposite side of reactor upper end is provided with chlorine ingress pipe，The discharging opening of reactor is connected with the charging aperture of steam tank by conveying pipe，The bottom of steam tank is provided with two discharging openings，One of them discharging opening is connected with exhaust gas absorption device，Another outlet is connected with the charging aperture of crude product tank；Fractionating device includes rectifying column and condenser, and the charging aperture of rectifying column is connected with the discharging opening of crude product tank, and the discharging opening of rectifying column is connected with the charging aperture of condenser by conveying pipe；Purifying plant includes crystallizer, fine work tank and rewinding tank, the charging aperture of crystallizer is connected with the discharging opening of condenser, the discharging opening of crystallizer is connected with the charging aperture of fine work tank, the bottom of fine work tank is provided with two discharging openings, one of them discharging opening is connected with rewinding tank, and another discharging opening is connected with exhaust gas absorption device；
Being additionally provided with corrosion-inhibiting coating on reactor inwall, 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=1:2；
First component includes following components according to the mass fraction: modifying epoxy resin by organosilicon: 25-31 part, pigment: 11-14 part, filler: 12-16 part, dispersant: 9-11 part, coalescents: 9-13 part, defoamer: 11-15 parts；
Second component includes following components according to the mass fraction: polyphenylene oxide resin powder: 18-20 part, toluene: 8-11 part, plasticizer: 5-8 part, coupling agent: 8-10 part, fire retardant: 2-7 part, compound rare-earth: 18-22 part；
Wherein, the one during pigment is titanium dioxide, white carbon black, barium sulfate or chrome oxide green；Filler glass flake or aluminium oxide one therein, dispersant is the one in sodium tetrapolyphosphate or sodium hexameta phosphate, and coalescents is the one in ethylene glycol, ethylene glycol or propylene glycol, and defoamer is organosilicon；
Plasticizer is the one in dioctyl phthalate or dibutyl phthalate, coupling agent is at least one in silane coupler or zirconium class coupling agent, fire retardant is phosphotriester, compound rare-earth includes following components by mass percentage: dysprosium: 15%, cerium: 22%, praseodymium: 4%, neodymium: 2%, remaining is lanthanum element, and above lanthanide rare each component sum is 100%.
The process units of aforesaid high-purity o chlorophenol, is provided with temperature sensor in storage tank and rewinding tank.
The process units of aforesaid high-purity o chlorophenol, the conveying pipe that rectifying column is connected with condenser is provided with metering device.
The process units of aforesaid high-purity o chlorophenol, is provided with heating tank in phenol preheater, in heating tank, installation is provided with and adds heat pipe, adds heat pipe and is isolated with phenol bucket by gripper shoe.
The process units of aforesaid high-purity o chlorophenol, is provided with agitator in reactor, agitator is double spiral agitator.
The process units of aforesaid high-purity o chlorophenol, the entrance point of chlorine ingress pipe and the port of export of exhaust gas absorption device are respectively equipped with valve.
The process units of aforesaid high-purity o chlorophenol, also includes the production technology of a kind of high-purity o chlorophenol, and 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 2-chlorophenol, 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 150-160 DEG C, continues stirring 15-20min and obtains mixed phenol；
Wherein, described 2-chlorophenol 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 175-180 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 o chlorophenol crystal after drying.
nullEmploying technical scheme provides the benefit that: be provided with phenol preheater in device，The complexity changing conventional device is heavy，Reduce the area occupied of device，The conveying pipe that rectifying column is connected with condenser and blue or green Liu Ta is connected with condenser is provided with metering device，Improve the purity of o-chlorphenol，This device is provided with exhaust gas absorption device，Avoid the discharge of waste gas，Thus protect environment，Improve work efficiency，The reactor corrosion-inhibiting coating suitability of present invention design is strong，Pollute little and low cost，Not only there is excellent damping，And there is stronger humidity and corrosion resistance，Reactor can be made unaffected in the case of being used for multiple times，Add the life-span of reactor，Decrease scrappage，And the production technology of o-chlorphenol is simple，Technique uses phenol as raw material，Reduce production cost，Protect environment，Improve work efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention；
Wherein: 1-storage tank, 2-phenol preheater, 3-reactor, 4-chlorine ingress pipe, 5-thermometer, 6-steam tank, 7-crude product tank, 8-exhaust gas absorption device, 9-rectifying column, 10-condenser, 11-crystallizer, 12-fine work tank, 13-rewinding tank.
Detailed description of the invention
Embodiment 1
nullThe present embodiment provides the process units of a kind of high-purity o chlorophenol，Including storage tank 1、Reaction unit、Exhaust gas absorption device 8、Fractionating device and purifying plant，Storage tank 1 is connected with reaction unit，Reaction unit includes phenol preheater 2、Reactor 3、Chlorine ingress pipe 4、Thermometer 5、Steam tank 6 and crude product tank 7，The side of storage tank 1 bottom is connected with the charging aperture of phenol preheater 2 by conveying pipe，The discharging opening of phenol preheater 2 is connected with the charging aperture of reactor 3 by conveying pipe，The side of reactor 3 upper end is provided with thermometer 5，The inside of reactor 3 is located in one end of thermometer 5，The opposite side of reactor 3 upper end is provided with chlorine ingress pipe 4，The discharging opening of reactor 3 is connected with the charging aperture of steam tank 6 by conveying pipe，The bottom of steam tank 6 is provided with two discharging openings，One of them discharging opening is connected with exhaust gas absorption device 8，Another outlet is connected with the charging aperture of crude product tank 7；Fractionating device includes rectifying column 9 and condenser 10, and the charging aperture of rectifying column 9 is connected with the discharging opening of crude product tank 7, and the discharging opening of rectifying column 9 is connected with the charging aperture of condenser 10 by conveying pipe；Purifying plant includes crystallizer 11, fine work tank 12 and rewinding tank 13, the charging aperture of crystallizer 11 is connected with the discharging opening of condenser 10, the discharging opening of crystallizer 11 is connected with the charging aperture of described fine work tank 12, the bottom of fine work tank 12 is provided with two discharging openings, one of them discharging opening is connected with rewinding tank 13, and another discharging opening is connected with exhaust gas absorption device 8；
Being additionally provided with corrosion-inhibiting coating on reactor 3 inwall, corrosion-inhibiting coating is formed on reactor 3 inwall by anti-corrosion paint, anticorrosive paint mixed by first and second liang of components, count first in mass ratio: second=1:2；
First component includes following components according to the mass fraction: modifying epoxy resin by organosilicon: 25 parts, pigment: 11 parts, filler: 12 parts, dispersant: 9 parts, coalescents: 9 parts, defoamer: 11 parts；
Second component includes following components according to the mass fraction: polyphenylene oxide resin powder: 18 parts, toluene: 8 parts, plasticizer: 5 parts, coupling agent: 8 parts, fire retardant: 2 parts, compound rare-earth: 18 parts；
Wherein, the one during pigment is titanium dioxide, white carbon black, barium sulfate or chrome oxide green；Filler glass flake or aluminium oxide one therein, dispersant is the one in sodium tetrapolyphosphate or sodium hexameta phosphate, and coalescents is the one in ethylene glycol, ethylene glycol or propylene glycol, and defoamer is organosilicon；
Plasticizer is the one in dioctyl phthalate or dibutyl phthalate, coupling agent is at least one in silane coupler or zirconium class coupling agent, fire retardant is phosphotriester, compound rare-earth includes following components by mass percentage: dysprosium: 15%, cerium: 22%, praseodymium: 4%, neodymium: 2%, remaining is lanthanum element, and above lanthanide rare each component sum is 100%；
Storage tank 1 and rewinding tank 13 are provided with temperature sensor, the conveying pipe that rectifying column 9 is connected with condenser 10 is provided with metering device, phenol preheater 2 is provided with heating tank, heating tank is installed to be provided with and adds heat pipe, add heat pipe to be isolated with phenol bucket by gripper shoe, being provided with agitator in reactor 3, agitator is double spiral agitator, and the entrance point of chlorine ingress pipe 4 and the port of export of exhaust gas absorption device 8 are respectively equipped with valve；
Also including the production technology of a kind of high-purity o chlorophenol, 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 2-chlorophenol, solvent and catalyst, then 20min is stirred, and it is gradually heated to 66 DEG C, open chlorine ingress pipe valve in reactor, be passed through chlorine, controlling into chlorine speed is that 15g/h makes chlorine add in 3h, and keeping the temperature within reactor is 150 DEG C, continues stirring 15min and obtains mixed phenol；
Wherein, described 2-chlorophenol 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 175 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 o chlorophenol crystal after drying.
Embodiment 2
nullThe present embodiment provides the process units of a kind of high-purity o chlorophenol，Including storage tank 1、Reaction unit、Exhaust gas absorption device 8、Fractionating device and purifying plant，Storage tank 1 is connected with reaction unit，Reaction unit includes phenol preheater 2、Reactor 3、Chlorine ingress pipe 4、Thermometer 5、Steam tank 6 and crude product tank 7，The side of storage tank 1 bottom is connected with the charging aperture of phenol preheater 2 by conveying pipe，The discharging opening of phenol preheater 2 is connected with the charging aperture of reactor 3 by conveying pipe，The side of reactor 3 upper end is provided with thermometer 5，The inside of reactor 3 is located in one end of thermometer 5，The opposite side of reactor 3 upper end is provided with chlorine ingress pipe 4，The discharging opening of reactor 3 is connected with the charging aperture of steam tank 6 by conveying pipe，The bottom of steam tank 6 is provided with two discharging openings，One of them discharging opening is connected with exhaust gas absorption device 8，Another outlet is connected with the charging aperture of crude product tank 7；Fractionating device includes rectifying column 9 and condenser 10, and the charging aperture of rectifying column 9 is connected with the discharging opening of crude product tank 7, and the discharging opening of rectifying column 9 is connected with the charging aperture of condenser 10 by conveying pipe；Purifying plant includes crystallizer 11, fine work tank 12 and rewinding tank 13, the charging aperture of crystallizer 11 is connected with the discharging opening of condenser 10, the discharging opening of crystallizer 11 is connected with the charging aperture of described fine work tank 12, the bottom of fine work tank 12 is provided with two discharging openings, one of them discharging opening is connected with rewinding tank 13, and another discharging opening is connected with exhaust gas absorption device 8；
Being additionally provided with corrosion-inhibiting coating on reactor 3 inwall, corrosion-inhibiting coating is formed on reactor 3 inwall by anti-corrosion paint, and anticorrosive paint is mixed by first and second liang of components, counts first in mass ratio: second=1:2；
First component includes following components according to the mass fraction: modifying epoxy resin by organosilicon: 31 parts, pigment: 14 parts, filler: 16 parts, dispersant: 11 parts, coalescents: 13 parts, defoamer: 15 parts；
Second component includes following components according to the mass fraction: polyphenylene oxide resin powder: 20 parts, toluene: 11 parts, plasticizer: 8 parts, coupling agent: 10 parts, fire retardant: 7 parts, compound rare-earth: 22 parts；
Wherein, the one during pigment is titanium dioxide, white carbon black, barium sulfate or chrome oxide green；Filler glass flake or aluminium oxide one therein, dispersant is the one in sodium tetrapolyphosphate or sodium hexameta phosphate, and coalescents is the one in ethylene glycol, ethylene glycol or propylene glycol, and defoamer is organosilicon；
Plasticizer is the one in dioctyl phthalate or dibutyl phthalate, coupling agent is at least one in silane coupler or zirconium class coupling agent, fire retardant is phosphotriester, compound rare-earth includes following components by mass percentage: dysprosium: 15%, cerium: 22%, praseodymium: 4%, neodymium: 2%, remaining is lanthanum element, and above lanthanide rare each component sum is 100%；
Storage tank 1 and rewinding tank 13 are provided with temperature sensor, the conveying pipe that rectifying column 9 is connected with condenser 10 is provided with metering device, phenol preheater 2 is provided with heating tank, heating tank is installed to be provided with and adds heat pipe, add heat pipe to be isolated with phenol bucket by gripper shoe, being provided with agitator in reactor 3, agitator is double spiral agitator, and the entrance point of chlorine ingress pipe 4 and the port of export of exhaust gas absorption device 8 are respectively equipped with valve；
Also including the production technology of a kind of high-purity o chlorophenol, 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 2-chlorophenol, solvent and catalyst, then 25min is stirred, and it is gradually heated to 70 DEG C, open chlorine ingress pipe valve in reactor, be passed through chlorine, controlling into chlorine speed is that 28g/h makes chlorine add in 5h, and keeping the temperature within reactor is 160 DEG C, continues stirring 20min and obtains mixed phenol；
Wherein, described 2-chlorophenol based on the amount ratio of material: chlorine: catalyst=1:1.8:0.005；
(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 180 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 o chlorophenol 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 (7)
- null1. the process units of a high-purity o chlorophenol，Including storage tank (1)、Reaction unit、Exhaust gas absorption device (8)、Fractionating device and purifying plant，It is characterized in that: described storage tank (1) is connected with reaction unit，Described reaction unit includes phenol preheater (2)、Reactor (3)、Chlorine ingress pipe (4)、Thermometer (5)、Steam tank (6) and crude product tank (7)，The side of described storage tank (1) bottom is connected with the charging aperture of described phenol preheater (2) by conveying pipe，The discharging opening of described phenol preheater (2) is connected with the charging aperture of reactor (3) by conveying pipe，The side of described reactor (3) upper end is provided with thermometer (5)，The inside of reactor (3) is located in one end of described thermometer (5)，The opposite side of described reactor (3) upper end is provided with chlorine ingress pipe (4)，The discharging opening of described reactor (3) is connected with the charging aperture of steam tank (6) by conveying pipe，The bottom of described steam tank (6) is provided with two discharging openings，One of them discharging opening described is connected with exhaust gas absorption device (8)，Another outlet is connected with the charging aperture of crude product tank (7)；Described fractionating device includes rectifying column (9) and condenser (10), the charging aperture of described rectifying column (9) is connected with the discharging opening of described crude product tank (7), and the discharging opening of described rectifying column (9) is connected with the charging aperture of condenser (10) by conveying pipe；Described purifying plant includes crystallizer (11), fine work tank (12) and rewinding tank (13), the charging aperture of described crystallizer (11) is connected with the discharging opening of described condenser (10), the discharging opening of described crystallizer (11) is connected with the charging aperture of described fine work tank (12), the bottom of described fine work tank (12) is provided with two discharging openings, one of them discharging opening described is connected with rewinding tank (13), and another discharging opening is connected with exhaust gas absorption device (8)；Being additionally provided with corrosion-inhibiting coating on described reactor (3) inwall, described corrosion-inhibiting coating is formed on reactor (3) inwall by anti-corrosion paint, and described anticorrosive paint is mixed by first and second liang of components, counts first in mass ratio: second=1:2；Described first component includes following components according to the mass fraction: modifying epoxy resin by organosilicon: 25-31 part, pigment: 11-14 part, filler: 12-16 part, dispersant: 9-11 part, coalescents: 9-13 part, defoamer: 11-15 parts；Described second component includes following components according to the mass fraction: polyphenylene oxide resin powder: 18-20 part, toluene: 8-11 part, plasticizer: 5-8 part, coupling agent: 8-10 part, fire retardant: 2-7 part, compound rare-earth: 18-22 part；Wherein, the one during described pigment is titanium dioxide, white carbon black, barium sulfate or chrome oxide green；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, and described defoamer is organosilicon；Described plasticizer is the one in dioctyl phthalate or dibutyl phthalate, described coupling agent is at least one in silane coupler or zirconium class coupling agent, described fire retardant is phosphotriester, described compound rare-earth includes following components by mass percentage: dysprosium: 15%, cerium: 22%, praseodymium: 4%, neodymium: 2%, remaining is lanthanum element, and above lanthanide rare each component sum is 100%.
- 2. according to the process units of the high-purity o chlorophenol described in claim 1, it is characterised in that: described storage tank (1) and rewinding tank (13) are provided with temperature sensor.
- 3. according to the process units of the high-purity o chlorophenol described in claim 1, it is characterised in that: the conveying pipe that described rectifying column (9) is connected with condenser (10) is provided with metering device.
- The process units of high-purity o chlorophenol the most according to claim 1, it is characterised in that: described phenol preheater (2) is provided with heating tank, described heating tank is installed and is provided with and adds heat pipe, described in add heat pipe and be isolated with phenol bucket by gripper shoe.
- The process units of high-purity o chlorophenol the most according to claim 1, it is characterised in that: being provided with agitator in described reactor (3), described agitator is double spiral agitator.
- The process units of high-purity o chlorophenol the most according to claim 1, it is characterised in that: the entrance point of described chlorine ingress pipe (4) and the port of export of exhaust gas absorption device (8) are respectively equipped with valve.
- 7. according to the process units of the high-purity o chlorophenol described in any claim in 1-6, it is characterised in that also including the production technology of a kind of high-purity o chlorophenol, 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 2-chlorophenol, 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 150-160 DEG C, continues stirring 15-20min and obtains mixed phenol；Wherein, described 2-chlorophenol 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 175-180 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 o chlorophenol crystal after drying.
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| CN201610296699.XA CN105906483A (en) | 2016-05-03 | 2016-05-03 | Production device and production process of high-purity o-chlorphenol |
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| CN201610296699.XA CN105906483A (en) | 2016-05-03 | 2016-05-03 | Production device and production process of high-purity o-chlorphenol |
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Citations (1)
| 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 |
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- 2016-05-03 CN CN201610296699.XA patent/CN105906483A/en active Pending
Patent Citations (1)
| 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 |
Non-Patent Citations (2)
| 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》 * |
| 陆友玲等: "邻、对氯苯酚残液的分离及利用", 《化学世界》 * |
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Application publication date: 20160831 |