CN106397157A - Method for preparing benzophenone - Google Patents
Method for preparing benzophenone Download PDFInfo
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- CN106397157A CN106397157A CN201610792424.5A CN201610792424A CN106397157A CN 106397157 A CN106397157 A CN 106397157A CN 201610792424 A CN201610792424 A CN 201610792424A CN 106397157 A CN106397157 A CN 106397157A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
- C07C45/46—Friedel-Crafts reactions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- 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
- Y02P20/141—Feedstock
Abstract
The invention discloses a method for preparing benzophenone. The method is characterized by comprising the following steps: (1) preparing materials, that is, adding benzene, quantitative catalysts and acyl chloride into a pre-reaction kettle, starting a condenser for cooling water, and stirring; (2) feeding, that is, conveying the prepared materials into a synthesis reactor by a feeding valve, wherein the pressure in the reactor is increased when the temperature of the synthesis reactor rises; (3) washing, and starting to stir and heat; (4) desolventizing, opening the feeding valve after receiving a washing station notification, feeding into a desolvation kettle, and closing the feeding valve after completing feeding; and (5) distilling, sucking the materials into a distillation mid-autoclave after desolvation, opening an air release valve of the distillation mid-autoclave, and regulating a mid-autoclave heating valve. The invention has the advantages that the preparation method has the advantages of simplicity, fewer byproducts, zero pollution and capacity of performing batch production.
Description
Technical field
The present invention relates to chemical technology field, especially relate to a kind of preparation method of benzophenone.
Background technology
Benzophenone, crystallizes for white glossiness prismatic.Resembling rose.Sweet taste.1G is dissolved in 7.5ml ethanol, 6ml second
Ether, is dissolved in chloroform, water insoluble.Relative density (d504) 1.0869.48.5 DEG C of fusing point.305.4 DEG C of boiling point.Index of refraction
(n45.2D)1.5975.138 DEG C of flash-point.Irritant, benzophenone be UV absorbent, organic pigment, medicine, spice,
The intermediate of insecticide.It is used in medical industry producing perhexiline, benztropine hydrobromate, diphenhydramine hydrochloride
Deng.This product is also styrene polymerization inhibitor and spice fixastive in itself.Essence can be given with sweet breath, used in multiple perfume
In fragrance for detergents.Can be used for allocating the edible essences such as Semen Armeniacae Amarum, Fructus Persicae, butter, Cortex cocois radiciss.Existing benzophenone synthetic route has
Phosgenation, Benzenecarbonyl chloride. method, carbon dioxide process, carbon monoxide method, benzoic acid (or benzoyl oxide) method, carbon tetrachloride method, catalysis
Oxidizing process, decarboxylation method etc..Wherein phosgenation, with phosgene and benzene as raw material, with lewis acid as catalyst, carries out Friedel-
Crafts react, through hydrolysis, layered shaping, refine etc. prepare benzophenone, present preparation method is loaded down with trivial details, and side-product is many.
Content of the invention
For overcoming the problems referred to above, the technical solution used in the present invention is as follows：
A kind of preparation method of benzophenone, step is as follows：
(1) get the raw materials ready, benzene, quantitative catalyst and acyl chlorides put in pre-reactor, opens condenser cooling water, open stirring,
Open steam and be warming up to 50 DEG C of stopping heating, keep 60 ± 3 DEG C of return stirrings 30 minutes, stop stirring pre-reaction and terminate；
(2) feed intake, will be got the raw materials ready by inlet valve and be delivered to synthesis reaction vessel, while synthesis reactor heats up, pressure in kettle
Can increase therewith.When pressure rises to 0.20Mpa, adjust conduction oil valve, turn-on flow rate meter air bleeding valve, all are checked to device
After normal, continue slow intensification.When pressure is slowly increased to 160 DEG C of 0.70～0.80MPa temperature, tune up air bleeding valve row further
Gas, by adjusting heat conduction fuel tap and air bleeding valve, strictly controls firing rate and capacity：Rise to 0.80～0.90Mpa in pressure,
During kettle temperature rises to 175 DEG C by 160 DEG C, heat up and slowly will be carried out with per hour 3～6 DEG C of speed；Rise to 1.15 in pressure
～1.35Mpa, during kettle temperature rises to 200 DEG C by 175 DEG C, programming rate is slowly carried out with per hour 4～7 DEG C of speed, when
Kettle temperature reaches 200～205 DEG C, when pressure reaches 1.30～1.35Mpa, insulation reaction to be continued 2 hours；
(3) wash, it is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, stir 10 minutes after reaching this temperature, stop
Stirring stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor；Upper strata feed liquid is stayed in kettle, continues
Add water about 1000L, and liquid level is up to position of platform.It is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, reaches this temperature
Stir 10 minutes afterwards, stop stirring stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor.
(4) precipitation, water receiving wash post notify after, open inlet valve, into precipitation kettle feed, after the completion of charging, close into
Material valve.Open heating valve, carry out normal pressure precipitation, when more water in glass trap, divide the water going below glass trap.
It is noted that firing rate, running audit relevant device and pipe fitting in heating process, find to turn down heating valve when having temperature too high
Door, prevents from condensing inadequate benzene evaporating into air.When being heated to 120 DEG C about, when reception flow is significantly smaller, can open and stir
Mix continuation normal pressure precipitation, when normal pressure precipitation flow is less, stops stirring, open WLW pump, carry out negative pressure precipitation.Beginning to use
It is necessary to according to receiving the slow Open valve of uninterrupted, just negative pressure can be gradually increased when flow is gradually little during negative pressure, until vacuum
Degree reaches more than -0.08MPa, standard-sized sheet vacuum valve, continues heating, opens stirring after substantially no after flow.When vacuum >=
0.08MPa, temperature >=130 DEG C, substantially no after flow, then open two stage pump by step, now vacuum answers >=0.09MPa, temperature
>=145 DEG C of degree, until substantially no after flow, crack bottom valve emptying, continues precipitation half an hour, after half an hour, stops stirring, close and steam
Steam valve door, crack atmospheric valve, close two stage pump, standard-sized sheet atmospheric valve, close WLW pump, adjust precipitation valve to normal pressure precipitation state.
Precipitation terminates.
(5) distill, after precipitation, material is sucked the middle kettle of distillation, open the atmospheric valve of kettle in the middle of distillation, adjust middle kettle
Heating valve, makes the temperature of charge of middle kettle control at 145 DEG C about；Control rectifying still temperature≤215 DEG C, tower top temperature≤195
DEG C, vacuum reaches -0.1Mpa.When needing to reduce tower top temperature, open tower top cooling water, control roof boiler temperature 55
～60 DEG C；Observe finished product and receive kettle reception and level condition, control finished product to receive the temperature of kettle material between 55～65 DEG C.Work as steaming
When evaporating that in kettle, content is relatively low, carry out the preparation to the charging of slag kettle；When relieving, to slowly open standby reception kettle vacuum valve,
After Vacuum Balance, open standby reception kettle splicing valve, close with kettle vacuum valve and splicing valve.
In described step (1), return stirring temperature is 60 DEG C.
In described step (2), programming rate is carried out with per hour 5 DEG C of speed.
Advantages of the present invention：Preparation method is simple now, and monitoring is convenient, shortens technological process, improves production efficiency,
Side-product is few, low cost, the pollution-free, advantage that can be mass.
Specific embodiment
A kind of preparation method of benzophenone, step is as follows：
(1) get the raw materials ready, benzene, quantitative catalyst and acyl chlorides put in pre-reactor, opens condenser cooling water, open stirring,
Open steam and be warming up to 50 DEG C of stopping heating, keep 60 ± 3 DEG C of return stirrings 30 minutes, stop stirring pre-reaction and terminate；
(2) feed intake, will be got the raw materials ready by inlet valve and be delivered to synthesis reaction vessel, while synthesis reactor heats up, pressure in kettle
Can increase therewith.When pressure rises to 0.20Mpa, adjust conduction oil valve, turn-on flow rate meter air bleeding valve, all are checked to device
After normal, continue slow intensification.When pressure is slowly increased to 160 DEG C of 0.70～0.80MPa temperature, tune up air bleeding valve row further
Gas, by adjusting heat conduction fuel tap and air bleeding valve, strictly controls firing rate and capacity：Rise to 0.80～0.90Mpa in pressure,
During kettle temperature rises to 175 DEG C by 160 DEG C, heat up and slowly will be carried out with per hour 3～6 DEG C of speed；Rise to 1.15 in pressure
～1.35Mpa, during kettle temperature rises to 200 DEG C by 175 DEG C, programming rate is slowly carried out with per hour 4～7 DEG C of speed, when
Kettle temperature reaches 200～205 DEG C, when pressure reaches 1.30～1.35Mpa, insulation reaction to be continued 2 hours；
(3) wash, it is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, stir 10 minutes after reaching this temperature, stop
Stirring stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor；Upper strata feed liquid is stayed in kettle, continues
Add water about 1000L, and liquid level is up to position of platform.It is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, reaches this temperature
Stir 10 minutes afterwards, stop stirring stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor.
(4) precipitation, water receiving wash post notify after, open inlet valve, into precipitation kettle feed, after the completion of charging, close into
Material valve.Open heating valve, carry out normal pressure precipitation, when more water in glass trap, divide the water going below glass trap.
It is noted that firing rate, running audit relevant device and pipe fitting in heating process, find to turn down heating valve when having temperature too high
Door, prevents from condensing inadequate benzene evaporating into air.When being heated to 120 DEG C about, when reception flow is significantly smaller, can open and stir
Mix continuation normal pressure precipitation, when normal pressure precipitation flow is less, stops stirring, open WLW pump, carry out negative pressure precipitation.Beginning to use
It is necessary to according to receiving the slow Open valve of uninterrupted, just negative pressure can be gradually increased when flow is gradually little during negative pressure, until vacuum
Degree reaches more than -0.08MPa, standard-sized sheet vacuum valve, continues heating, opens stirring after substantially no after flow.When vacuum >=
0.08MPa, temperature >=130 DEG C, substantially no after flow, then open two stage pump by step, now vacuum answers >=0.09MPa, temperature
>=145 DEG C of degree, until substantially no after flow, crack bottom valve emptying, continues precipitation half an hour, after half an hour, stops stirring, close and steam
Steam valve door, crack atmospheric valve, close two stage pump, standard-sized sheet atmospheric valve, close WLW pump, adjust precipitation valve to normal pressure precipitation state.
Precipitation terminates.
(5) distill, after precipitation, material is sucked the middle kettle of distillation, open the atmospheric valve of kettle in the middle of distillation, adjust middle kettle
Heating valve, makes the temperature of charge of middle kettle control at 145 DEG C about；Control rectifying still temperature≤215 DEG C, tower top temperature≤195
DEG C, vacuum reaches -0.1Mpa.When needing to reduce tower top temperature, open tower top cooling water, control roof boiler temperature 55
～60 DEG C；Observe finished product and receive kettle reception and level condition, control finished product to receive the temperature of kettle material between 55～65 DEG C.Work as steaming
When evaporating that in kettle, content is relatively low, carry out the preparation to the charging of slag kettle；When relieving, to slowly open standby reception kettle vacuum valve,
After Vacuum Balance, open standby reception kettle splicing valve, close with kettle vacuum valve and splicing valve.
In described step (1), return stirring temperature is 60 DEG C.
In described step (2), programming rate is carried out with per hour 5 DEG C of speed.
Embodiment 1
A kind of preparation method of benzophenone, step is as follows：
(1) get the raw materials ready, benzene, quantitative catalyst and acyl chlorides put in pre-reactor, opens condenser cooling water, open stirring,
Open steam and be warming up to 50 DEG C of stopping heating, keep 60 DEG C of return stirrings 30 minutes, stop stirring pre-reaction and terminate；
(2) feed intake, will be got the raw materials ready by inlet valve and be delivered to synthesis reaction vessel, while synthesis reactor heats up, pressure in kettle
Can increase therewith.When pressure rises to 0.20Mpa, adjust conduction oil valve, turn-on flow rate meter air bleeding valve, all are checked to device
After normal, continue slow intensification.When pressure is slowly increased to 160 DEG C of 0.70～0.80MPa temperature, tune up air bleeding valve row further
Gas, by adjusting heat conduction fuel tap and air bleeding valve, strictly controls firing rate and capacity：Rise to 0.80～0.90Mpa in pressure,
During kettle temperature rises to 175 DEG C by 160 DEG C, heat up and slowly will be carried out with per hour 5 DEG C of speed；Rise to 1.15 in pressure～
1.35Mpa, during kettle temperature rises to 200 DEG C by 175 DEG C, programming rate is slowly carried out with per hour 4～7 DEG C of speed, works as kettle
Temperature reaches 200～205 DEG C, when pressure reaches 1.30～1.35Mpa, insulation reaction to be continued 2 hours；
(3) wash, it is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, stir 10 minutes after reaching this temperature, stop
Stirring stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor；Upper strata feed liquid is stayed in kettle, continues
Add water about 1000L, and liquid level is up to position of platform.It is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, reaches this temperature
Stir 10 minutes afterwards, stop stirring stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor.
(4) precipitation, water receiving wash post notify after, open inlet valve, into precipitation kettle feed, after the completion of charging, close into
Material valve.Open heating valve, carry out normal pressure precipitation, when more water in glass trap, divide the water going below glass trap.
It is noted that firing rate, running audit relevant device and pipe fitting in heating process, find to turn down heating valve when having temperature too high
Door, prevents from condensing inadequate benzene evaporating into air.When being heated to 120 DEG C about, when reception flow is significantly smaller, can open and stir
Mix continuation normal pressure precipitation, when normal pressure precipitation flow is less, stops stirring, open WLW pump, carry out negative pressure precipitation.Beginning to use
It is necessary to according to receiving the slow Open valve of uninterrupted, just negative pressure can be gradually increased when flow is gradually little during negative pressure, until vacuum
Degree reaches more than -0.08MPa, standard-sized sheet vacuum valve, continues heating, opens stirring after substantially no after flow.When vacuum >=
0.08MPa, temperature >=130 DEG C, substantially no after flow, then open two stage pump by step, now vacuum answers >=0.09MPa, temperature
>=145 DEG C of degree, until substantially no after flow, crack bottom valve emptying, continues precipitation half an hour, after half an hour, stops stirring, close and steam
Steam valve door, crack atmospheric valve, close two stage pump, standard-sized sheet atmospheric valve, close WLW pump, adjust precipitation valve to normal pressure precipitation state.
Precipitation terminates.
(5) distill, after precipitation, material is sucked the middle kettle of distillation, open the atmospheric valve of kettle in the middle of distillation, adjust middle kettle
Heating valve, makes the temperature of charge of middle kettle control at 145 DEG C about；Control rectifying still temperature≤215 DEG C, tower top temperature≤195
DEG C, vacuum reaches -0.1Mpa.When needing to reduce tower top temperature, open tower top cooling water, control roof boiler temperature 55
～60 DEG C；Observe finished product and receive kettle reception and level condition, control finished product to receive the temperature of kettle material between 55～65 DEG C.Work as steaming
When evaporating that in kettle, content is relatively low, carry out the preparation to the charging of slag kettle；When relieving, to slowly open standby reception kettle vacuum valve,
After Vacuum Balance, open standby reception kettle splicing valve, close with kettle vacuum valve and splicing valve.
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and any
Those of ordinary skill in the art disclosed herein technical scope in, the change or replacement that can readily occur in, all should contain
Cover within protection scope of the present invention.Therefore, the protection model that protection scope of the present invention should be limited with claims
Enclose and be defined.
Claims (3)
1. a kind of preparation method of benzophenone is it is characterised in that step is as follows：
(1) get the raw materials ready, benzene, quantitative catalyst and acyl chlorides are put in pre-reactor, opens condenser cooling water, open stirring, open
Steam is warming up to 50 DEG C and stops heating, keeps 60 ± 3 DEG C of return stirrings 30 minutes, stops stirring pre-reaction and terminates；
(2) feed intake, will be got the raw materials ready by inlet valve and be delivered to synthesis reaction vessel, while synthesis reactor heats up, in kettle, pressure can be with
Increase.When pressure rises to 0.20Mpa, adjust conduction oil valve, turn-on flow rate meter air bleeding valve, device inspection is all gone well
Afterwards, continue slow intensification.When pressure is slowly increased to 160 DEG C of 0.70～0.80MPa temperature, tune up aerofluxuss valve exhaust further,
By adjusting heat conduction fuel tap and air bleeding valve, strictly control firing rate and capacity：Rise to 0.80～0.90Mpa, kettle in pressure
During temperature rises to 175 DEG C by 160 DEG C, heat up and slowly will be carried out with per hour 3～6 DEG C of speed；Rise to 1.15 in pressure～
1.35Mpa, during kettle temperature rises to 200 DEG C by 175 DEG C, programming rate is slowly carried out with per hour 4～7 DEG C of speed, works as kettle
Temperature reaches 200～205 DEG C, when pressure reaches 1.30～1.35Mpa, insulation reaction to be continued 2 hours；
(3) wash, it is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, stir 10 minutes after reaching this temperature, stop stirring
Stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor；Upper strata feed liquid is stayed in kettle, continues to add water
About 1000L, liquid level is up to position of platform.It is 53～57 DEG C that unlatching stirring, heating valve make temperature in the kettle, stirs after reaching this temperature
Mix 10 minutes, stop stirring stratification 10 minutes, opening washing kettle lower valve makes water layer enter sour water oil interceptor.
(4) precipitation, after water receiving washes post notice, opens inlet valve, feeds into precipitation kettle, after the completion of charging, closes inlet valve.
Open heating valve, carry out normal pressure precipitation, when more water in glass trap, divide the water going below glass trap.Heating
During it is noted that firing rate, running audit relevant device and pipe fitting, find to turn down heating valve when having temperature too high, prevent
Only condense inadequate benzene and evaporate into air.When being heated to 120 DEG C about, when reception flow is significantly smaller, stirring can be opened and continue
Continuous normal pressure precipitation, when normal pressure precipitation flow is less, stops stirring, opens WLW pump, carry out negative pressure precipitation.Beginning to use negative pressure
When it is necessary to according to receiving the slow Open valve of uninterrupted, just negative pressure can be gradually increased when flow is gradually little, until vacuum reaches
Arrive more than -0.08MPa, standard-sized sheet vacuum valve, continue heating, open stirring after substantially no after flow.As vacuum >=0.08MPa,
Temperature >=130 DEG C, substantially no after flow, then open two stage pump by step, now vacuum answers >=0.09MPa, temperature >=145
DEG C, until substantially no after flow, crack bottom valve emptying, continue precipitation half an hour, after half an hour, stop stirring, steam off valve,
Crack atmospheric valve, cuts out two stage pump, standard-sized sheet atmospheric valve, cuts out WLW pump, adjusts precipitation valve to normal pressure precipitation state.Precipitation is tied
Bundle.
(5) distill, after precipitation, material is sucked the middle kettle of distillation, open the atmospheric valve of kettle in the middle of distillation, adjust middle kettle heating
Valve, makes the temperature of charge of middle kettle control at 145 DEG C about；Control rectifying still temperature≤215 DEG C, tower top temperature≤195 DEG C, very
Reciprocal of duty cycle reaches -0.1Mpa.When needing to reduce tower top temperature, open tower top cooling water, control roof boiler temperature 55～60
℃；Observe finished product and receive kettle reception and level condition, control finished product to receive the temperature of kettle material between 55～65 DEG C.Work as distillating still
When interior content is relatively low, carry out the preparation to the charging of slag kettle；When relieving, to slowly open standby reception kettle vacuum valve, treat true
After empty balance, open standby reception kettle splicing valve, close with kettle vacuum valve and splicing valve.
2. a kind of benzophenone according to claim 1 preparation method it is characterised in that：Backflow in described step (1)
Whipping temp is 60 DEG C.
3. a kind of benzophenone according to claim 1 preparation method it is characterised in that：Heat up in described step (2)
Speed is carried out with per hour 5 DEG C of speed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610792424.5A CN106397157A (en) | 2016-08-31 | 2016-08-31 | Method for preparing benzophenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610792424.5A CN106397157A (en) | 2016-08-31 | 2016-08-31 | Method for preparing benzophenone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106397157A true CN106397157A (en) | 2017-02-15 |
Family
ID=58001957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610792424.5A Pending CN106397157A (en) | 2016-08-31 | 2016-08-31 | Method for preparing benzophenone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115448828A (en) * | 2022-09-23 | 2022-12-09 | 重庆长风化学工业有限公司 | Production process of benzophenone and safe working method in production process |
-
2016
- 2016-08-31 CN CN201610792424.5A patent/CN106397157A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115448828A (en) * | 2022-09-23 | 2022-12-09 | 重庆长风化学工业有限公司 | Production process of benzophenone and safe working method in production process |
| CN115448828B (en) * | 2022-09-23 | 2023-11-10 | 重庆长风化学工业有限公司 | Production process of diphenyl ketone and safe working method in process |
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Application publication date: 20170215 |