CN108191641A - A kind of recovery and treatment method of chlorobenzoyl chloride raffinate - Google Patents
A kind of recovery and treatment method of chlorobenzoyl chloride raffinate Download PDFInfo
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- CN108191641A CN108191641A CN201810016105.4A CN201810016105A CN108191641A CN 108191641 A CN108191641 A CN 108191641A CN 201810016105 A CN201810016105 A CN 201810016105A CN 108191641 A CN108191641 A CN 108191641A
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- chlorobenzoyl chloride
- vacuum distillation
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- raffinate
- distillation plant
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- Water Supply & Treatment (AREA)
- Crystallography & Structural Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a kind of recovery and treatment methods of chlorobenzoyl chloride raffinate, include the following steps, chlorobenzoyl chloride raffinate is subjected to vacuum distillation processing first, and it carries out being condensed back to receipts chlorobenzoyl chloride, secondly basic hydrolysis processing is carried out to remaining chlorobenzoyl chloride raffinate, tasteless chlorobenzoyl chloride treatment fluid is obtained after the completion of processing, chlorobenzoyl chloride treatment fluid is finally discharged into vacuum distillation plant, it is cooled to room temperature rear spontaneous curing, the chlorobenzoyl chloride rate of recovery purity of the program is high, the rate of recovery is high, treatment process is simple to operation, and treated that solid residue has no irritating odor, convenient for being routed directly to qualified dangerous waste processing company processing, safety and environmental protection.
Description
Technical field
The present invention relates to chlorobenzoyl chloride production fields, are specifically related to a kind of recovery and treatment method of chlorobenzoyl chloride raffinate.
Background technology
Chlorobenzoyl chloride, colourless liquid, irritant smell, chlorobenzoyl chloride for prepare dyestuff, fragrance, organic peroxide,
The important intermediate of drug and resin, chlorobenzoyl chloride are important benzoylation and benzylating reagent.Most of chlorobenzoyl chloride is used
Benzoyl peroxide is produced, secondly for the important of production benzophenone, Ergol, benzylcellulose and benzamide etc.
Industrial chemicals;Chlorobenzoyl chloride has eyes, mucocutaneous and respiratory tract strong impulse effect, and sucking may be due to larynx, branch gas
The spasm of pipe, oedema, inflammation, chemical pneumonia, pulmonary edema and it is lethal.It meets open fire, high fever or is contacted with oxidant, have and cause combustion
The danger that decrepitate is fried meets water reaction fever and releases toxic corrosive gas, in the presence of many metals especially humid air
It is corrosive;The synthesis technology of chlorobenzoyl chloride mainly has toluene method, phosgenation, benzoic acid silicon tetrachloride method etc., due to raw material and
The influence of synthesis technology, chlorobenzoyl chloride production process generate raffinate in still have a large amount of chlorobenzoyl chlorides and other noxious materials,
With strong impulse smell, direct emission is very big to environment and human health damage, in the prior art, is prepared by toluene method
In chlorobenzoyl chloride technique, chlorobenzoyl chloride raffinate processing method is mostly to turn chlorobenzoyl chloride in residual night by the methods of distillation, synthesis
Benzoic acid is turned to, this method complex process, the benzoic acid of recycling can not be reused as product, in addition, the prior art is also deposited
Recycling purity is low, the problem of treated residue inconvenience conveying and storage.
Invention content
In view of the deficiencies of the prior art, the technical problem to be solved in the present invention is to provide a kind of recycling of chlorobenzoyl chloride raffinate
Processing method, the chlorobenzoyl chloride purity of the recycling of the program is high, and production cost, treatment process have been saved while can reusing
It is simple to operation, and treated that solid residue has no irritating odor, convenient for being routed directly at qualified dangerous waste processing company
Reason, safety and environmental protection.
To solve the above problems, the present invention provides following technical solutions:A kind of recovery processing side of chlorobenzoyl chloride raffinate
Method, which is characterized in that include the following steps:
(1)Heating in vacuum is distilled
Chlorobenzoyl chloride raffinate is placed in vacuum distillation plant, temperature is 115-125 DEG C, vacuum degree is 0.08-0.1MPa items
Heating in vacuum distillation is carried out under part;
In vacuum distillation process, the chlorobenzoyl chloride in chlorobenzoyl chloride raffinate is at high temperature and under vacuum action, and boiling point reduces, benzene first
Acyl chlorides is evaporated with gaseous state.
(2)Condensation recycling
By the outlet side of vacuum distillation plant and condenser unicom, step(1)The condensed device of retort gas that heating distillation obtains
Cooling recycling obtains chlorobenzoyl chloride;
Condensation process, find condenser recycling benzoyl chlorine dose reduce to no liquid chlorobenzoyl chloride generates when, heating in vacuum steaming
Evaporating step can stop.
(3)Basic hydrolysis
Into vacuum distillation plant be added dropwise alkali process agent, keep vacuum distillation plant in temperature be 130-150 DEG C, vacuum degree is
0.02-0.06MPa, is hydrolyzed reaction, obtains chlorobenzoyl chloride treatment fluid after reaction;
Hydrolytic process can make after vacuum distillation micro chlorobenzoyl chloride in remaining raffinate, benzoic acid, benzotrichloride basic hydrolysis into
Organic salt, and then thoroughly eliminate residual chlorobenzoyl chloride.Atomization hydrogen chloride gas, chlorine can be generated in hydrolytic process vacuum distillation plant
Change hydrogen to discharge by vacuum distillation plant outlet side, when the atomization gas of device to be seen fades away, hydrolysis knot
Beam.
(4)Residue cures
Rate-determining steps(3)Middle chlorobenzoyl chloride treatment fluid temperature is 115-125 DEG C, by chlorobenzoyl chloride treatment fluid from vacuum distillation plant
In draw off, after being cooled to room temperature, obtain the chlorobenzoyl chloride residue of solid.
After temperature reduces, the state of chlorobenzoyl chloride treatment fluid gradually becomes thick, you can is drawn off, such as temperature mistake
Low, chlorobenzoyl chloride will be caused to handle, and fluid viscosity is excessive, and inconvenience is drawn off.
The main component of chlorobenzoyl chloride treatment fluid is organic salt, phenyl ring chloride, catalyst and high-boiling components, is down to room temperature
Afterwards, become solid from thick in the chlorobenzoyl chloride treatment fluid being made of substantially high polymer, it is tasteless, convenient for having sent at qualification dangerous waste
Reason company is handled.
Preferably, the step(1)In, the vacuum degree of heating in vacuum distillation is not less than 0.085MPa.
Preferably, the step(3)In, the vacuum degree of vacuum distillation plant is 0.04MPa.
Technical scheme of the present invention further includes, and the alkali process agent is sodium hydroxide solution, one kind of potassium hydroxide solution.
Preferably, the alkali process agent is sodium hydroxide solution, a concentration of 25%-32% of sodium hydroxide solution.
Technical scheme of the present invention further includes, the step(3)In, alkali process agent is added in into vacuum distillation plant, and
It is stirred at 150 DEG C, until being generated in vacuum distillation plant without atomization gas, hydrolysis is completed, and stops adding alkali process
Temperature in vacuum distillation plant is down to 120 DEG C by agent, stands 0.5-1h, and chlorobenzoyl chloride treatment fluid is drawn off in after thick.
Technical scheme of the present invention further includes, the step(3)In, the exhaust gas that basic hydrolysis generates is by being placed in vacuum distillation
The water spray equipment of device outlet side absorbs.
The beneficial effects of the invention are as follows:The object of the present invention is to provide a kind of chlorobenzoyl chloride organic efficiency height, treatment process
Chlorobenzoyl chloride raffinate recovery and treatment method that is simple and being convenient for Slag recovering processing after processing, compared with prior art, this programme
Chlorobenzoyl chloride raffinate is recycled by vacuum distillation method, the chlorobenzoyl chloride purity after recycling is more than 97.5%, can directly throw
Enter to use, saved production cost, the rate of recovery of chlorobenzoyl chloride is more than 50%;By basic hydrolysis technique, will be remained after vacuum distillation
Residue in remaining raffinate is hydrolyzed to tasteless organic salt, phenyl ring chloride, catalyst and high-boiling components etc., thoroughly eliminates benzene first
Acyl chlorides after the completion of basic hydrolysis, the chlorobenzoyl chloride treatment fluid after hydrolysis out of vacuum distillation plant is drawn off, is cured after cooling,
Convenient for having sent the processing of qualification dangerous waste processing company, entire recovery processing process is simple, and non-secondary pollution is easy to operation, peace
Loopful is protected.
Specific embodiment
With reference to embodiment, technical scheme of the present invention is described in detail, the chlorobenzoyl chloride described in this programme
Raffinate obtains after producing chlorobenzoyl chloride by toluene method.
Embodiment 1
A kind of recovery and treatment method of chlorobenzoyl chloride raffinate, includes the following steps:
(1)Heating in vacuum is distilled
1900Kg chlorobenzoyl chloride raffinates are placed in vacuum distillation plant, temperature is 115 DEG C, vacuum degree is 0.08MPa conditions
Lower progress heating in vacuum distillation.
(2)Condensation recycling
By the outlet side of vacuum distillation plant and condenser unicom, step(1)The condensed device of retort gas that heating distillation obtains
Cooling recycling obtains chlorobenzoyl chloride, weighs, records;
Condensation process, find condenser recycling benzoyl chlorine dose reduce to no liquid chlorobenzoyl chloride generates when, heating in vacuum steaming
Evaporating step can stop.
(3)Basic hydrolysis
Into vacuum distillation plant be added dropwise alkali process agent, keep vacuum distillation plant in temperature be 130 DEG C, vacuum degree is
0.02MPa is hydrolyzed reaction, can generate atomization hydrogen chloride gas in hydrolytic process vacuum distillation plant, hydrogen chloride gas leads to
The discharge of vacuum distillation plant outlet side is crossed, when the atomization gas of device to be seen fades away, hydrolysis terminates, and obtains benzene first
Acyl chlorides treatment fluid.
(4)Residue cures
Rate-determining steps(3)Middle chlorobenzoyl chloride treatment fluid temperature is 120 DEG C, by thick chlorobenzoyl chloride treatment fluid from vacuum distillation
It is drawn off in device, after being cooled to room temperature, obtains the chlorobenzoyl chloride residue of solid, weigh and record.
Chlorobenzoyl chloride residue is tasteless, convenient for having sent the processing of qualification dangerous waste processing company.
Embodiment 2
A kind of recovery and treatment method of chlorobenzoyl chloride raffinate, includes the following steps:
(1)Heating in vacuum is distilled
1900Kg chlorobenzoyl chloride raffinates are placed in vacuum distillation plant, temperature is 125 DEG C, vacuum degree is 0.085MPa conditions
Lower progress heating in vacuum distillation.
(2)Condensation recycling
By the outlet side of vacuum distillation plant and condenser unicom, step(1)The condensed device of retort gas that heating distillation obtains
Cooling recycling obtains chlorobenzoyl chloride, weighs, records;
Condensation process, find condenser recycling benzoyl chlorine dose reduce to no liquid chlorobenzoyl chloride generates when, heating in vacuum steaming
Evaporating step can stop.
(3)Basic hydrolysis
Into vacuum distillation plant be added dropwise alkali process agent, keep vacuum distillation plant in temperature be 150 DEG C, vacuum degree is
0.04MPa is hydrolyzed reaction, can generate atomization hydrogen chloride gas in hydrolytic process vacuum distillation plant, hydrogen chloride gas leads to
The discharge of vacuum distillation plant outlet side is crossed, when the atomization gas of device to be seen fades away, hydrolysis terminates, and obtains benzene first
Acyl chlorides treatment fluid.
(4)Residue cures
Rate-determining steps(3)Middle chlorobenzoyl chloride treatment fluid temperature is 120 DEG C, by thick chlorobenzoyl chloride treatment fluid from vacuum distillation
It is drawn off in device, after being cooled to room temperature, obtains the chlorobenzoyl chloride residue of solid, weigh and record.
Chlorobenzoyl chloride residue is tasteless, convenient for having sent the processing of qualification dangerous waste processing company.
Embodiment 3
A kind of recovery and treatment method of chlorobenzoyl chloride raffinate, includes the following steps:
(1)Heating in vacuum is distilled
1900Kg chlorobenzoyl chloride raffinates are placed in vacuum distillation plant, under the conditions of temperature is 120 DEG C, vacuum degree is 0.1MPa
Carry out heating in vacuum distillation.
(2)Condensation recycling
By the outlet side of vacuum distillation plant and condenser unicom, step(1)The condensed device of retort gas that heating distillation obtains
Cooling recycling obtains chlorobenzoyl chloride, weighs, records;
Condensation process, find condenser recycling benzoyl chlorine dose reduce to no liquid chlorobenzoyl chloride generates when, heating in vacuum steaming
Evaporating step can stop.
(3)Basic hydrolysis
Into vacuum distillation plant be added dropwise alkali process agent, keep vacuum distillation plant in temperature be 140 DEG C, vacuum degree is
0.06MPa is hydrolyzed reaction, can generate atomization hydrogen chloride gas in hydrolytic process vacuum distillation plant, hydrogen chloride gas leads to
The discharge of vacuum distillation plant outlet side is crossed, when the atomization gas of device to be seen fades away, hydrolysis terminates, and obtains benzene first
Acyl chlorides treatment fluid.
(4)Residue cures
Rate-determining steps(3)Middle chlorobenzoyl chloride treatment fluid temperature is 120 DEG C, by thick chlorobenzoyl chloride treatment fluid from vacuum distillation
It is drawn off in device, after being cooled to room temperature, obtains the chlorobenzoyl chloride residue of solid, weigh and record.
Chlorobenzoyl chloride residue is tasteless, convenient for having sent the processing of qualification dangerous waste processing company.
The various embodiments described above chlorobenzoyl chloride raffinate handling result is as shown in table 1.
1 each embodiment chlorobenzoyl chloride raffinate handling result of table
Raffinate quality/kg | Recycle chlorobenzoyl chloride quality/kg | Recycle chlorobenzoyl chloride purity/% | Chlorobenzoyl chloride mass of residue/kg | The rate of recovery/% | |
Embodiment 1 | 1900 | 980 | 97.9 | 810 | 51.2 |
Embodiment 2 | 1900 | 1052 | 98.2 | 800 | 55.4 |
Embodiment 3 | 1900 | 1130 | 97.8 | 803 | 59.5 |
Each embodiment test data of upper table shows, chlorobenzoyl chloride raffinate recovery and treatment method of the invention, the chlorobenzoyl chloride rate of recovery
More than 50%, and the chlorobenzoyl chloride purity recycled is high, convenient for recycling, while has prevented to remain chlorobenzoyl chloride etc. in residue and has
Harm of the noxious material to environment and health.
Protection scope of the present invention is not limited only to examples detailed above, after the present invention has been read, those skilled in the art couple
The modification of the various same principles of the present invention falls within the attached claim limited range of the application.
Claims (7)
1. a kind of recovery and treatment method of chlorobenzoyl chloride raffinate, which is characterized in that include the following steps:
(1)Heating in vacuum is distilled
Chlorobenzoyl chloride raffinate is placed in vacuum distillation plant, temperature is 115-125 DEG C, vacuum degree is 0.08-0.1MPa items
Heating in vacuum distillation is carried out under part;
(2)Condensation recycling
By the outlet side of vacuum distillation plant and condenser unicom, step(1)The condensed device of retort gas that heating distillation obtains
Cooling recycling obtains chlorobenzoyl chloride;
(3)Basic hydrolysis
Into vacuum distillation plant be added dropwise alkali process agent, keep vacuum distillation plant in temperature be 130-150 DEG C, vacuum degree is
0.02-0.06MPa, is hydrolyzed reaction, obtains chlorobenzoyl chloride treatment fluid after reaction;
(4)Residue cures
Rate-determining steps(3)Middle chlorobenzoyl chloride treatment fluid temperature is 115-125 DEG C, by chlorobenzoyl chloride treatment fluid from vacuum distillation plant
In draw off, after being cooled to room temperature, obtain the chlorobenzoyl chloride residue of solid.
2. the recovery and treatment method of chlorobenzoyl chloride raffinate as described in claim 1, it is characterised in that:The step(1)In, very
The vacuum degree of sky heating distillation is not less than 0.085MPa.
3. the recovery and treatment method of chlorobenzoyl chloride raffinate as described in claim 1, it is characterised in that:The step(3)In, very
The vacuum degree of empty distilling apparatus is 0.04MPa.
4. the recovery and treatment method of chlorobenzoyl chloride raffinate as described in claim 1, it is characterised in that:The alkali process agent is hydrogen
Sodium hydroxide solution, one kind of potassium hydroxide solution.
5. the recovery and treatment method of chlorobenzoyl chloride raffinate as described in claim 1, it is characterised in that:The alkali process agent is hydrogen
Sodium hydroxide solution, a concentration of 25%-32% of sodium hydroxide solution.
6. the recovery and treatment method of chlorobenzoyl chloride raffinate as described in claim 1, it is characterised in that:The step(3)In, to
Alkali process agent is added in vacuum distillation plant, and is stirred at 150 DEG C, until being produced in vacuum distillation plant without atomization gas
Raw, hydrolysis is completed, and stops adding alkali process agent, and temperature in vacuum distillation plant is down to 120 DEG C, stands 0.5-1h, benzene
Formyl chloride treatment fluid is drawn off in after thick.
7. the recovery and treatment method of chlorobenzoyl chloride raffinate as described in claim 1, it is characterised in that:The step(3)In, alkali
Property hydrolysis generate exhaust gas by be placed in vacuum distillation plant outlet side water spray equipment absorb.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110963910A (en) * | 2019-12-17 | 2020-04-07 | 南通市天时化工有限公司 | Method for vacuum system in process of preparing acyl chloride by benzal chloride acidolysis method |
CN112759163A (en) * | 2020-12-31 | 2021-05-07 | 清大国华环境集团股份有限公司 | Treatment method and treatment system for residual liquid generated in benzoyl chloride production process |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105175242A (en) * | 2015-09-14 | 2015-12-23 | 宜都市友源实业有限公司 | Method for recycling trichlorotoluene and/or benzoyl chloride waste slag |
CN205662478U (en) * | 2016-06-03 | 2016-10-26 | 宜都市友源实业有限公司 | Benzoyl chloride distills residual material recovery unit |
-
2018
- 2018-01-08 CN CN201810016105.4A patent/CN108191641A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105175242A (en) * | 2015-09-14 | 2015-12-23 | 宜都市友源实业有限公司 | Method for recycling trichlorotoluene and/or benzoyl chloride waste slag |
CN205662478U (en) * | 2016-06-03 | 2016-10-26 | 宜都市友源实业有限公司 | Benzoyl chloride distills residual material recovery unit |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110963910A (en) * | 2019-12-17 | 2020-04-07 | 南通市天时化工有限公司 | Method for vacuum system in process of preparing acyl chloride by benzal chloride acidolysis method |
CN112759163A (en) * | 2020-12-31 | 2021-05-07 | 清大国华环境集团股份有限公司 | Treatment method and treatment system for residual liquid generated in benzoyl chloride production process |
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Application publication date: 20180622 |