CN106748691A - The process for producing of benzophenone - Google Patents
The process for producing of benzophenone Download PDFInfo
- Publication number
- CN106748691A CN106748691A CN201611127957.8A CN201611127957A CN106748691A CN 106748691 A CN106748691 A CN 106748691A CN 201611127957 A CN201611127957 A CN 201611127957A CN 106748691 A CN106748691 A CN 106748691A
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- CN
- China
- Prior art keywords
- benzophenone
- rectifying column
- producing
- rectifying
- added
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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
-
- 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
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
The present invention provides a kind of process for producing of benzophenone, and operating procedure is as follows：1) dry benzene is added in the retort for being added with chlorobenzoyl chloride, and catalyst alchlor is added under agitation, and imported into reaction solution in frozen water and is layered by heating reflux reaction, oil reservoir is taken by drying, depressurizing, be fractionated, crystallize, dry, thick benzophenone is obtained；2) by step 1) prepare thick benzophenone be placed in rectifying column, 170 185 DEG C are heated under reduced pressure；3) step 2) in rectifying column rectifying terminal for rectifying column tower temperature be 220 230 DEG C.By the way that first benzene is reacted with chlorobenzoyl chloride, prepare thick benzophenone, overcome the difference of different because of raw material sources from production technology, impurity can be produced, then rectifying column distillation operation is passed through, the high-quality benzophenone of high-purity (purity ＞ 99.89%) can be obtained, while spy controls the prepared composition of whole technique, application can be further generalized in actual industrial production.
Description
Technical field
The present invention relates to benzophenone production field, and in particular to a kind of process for producing of benzophenone.
Background technology
Continued to develop with now industrialized, people, also can be for quality of the life while living standard is lifted
More and more higher is pursued, especially for the use of daily chemical product.
Benzophenone is the intermediate of ultra-violet absorber, organic pigment, medicine, spices, insecticide.Used in medical industry
In production perhexiline, benzatropine hydrobromate, diphenhydramine hydrochloride etc..This product is also in itself that styrene polymerization suppresses
Agent and spices fixastive.Essence can be assigned with sweet breath, in various perfume and fragrance for detergents.Can be used for allocate almond,
The flavoring essences such as peach, cream, coconut.
It is widely used in life just because of benzophenone so that the production quality requirement for benzophenone is also more next
Higher, in present traditional handicraft preparation process, the refined yield of production benzophenone is low, has had a strong impact on its benzophenone
Use and promote.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of process for producing of benzophenone so that hexichol first
The preparation purity of ketone is further lifted.
To realize object above, the present invention is achieved by the following technical programs：
A kind of process for producing of benzophenone, operating procedure is as follows：
1) dry benzene is added in the retort for being added with chlorobenzoyl chloride, and adds catalyst under agitation
Imported into reaction solution in frozen water and be layered by alchlor, heating reflux reaction, take oil reservoir by drying, decompression, fractionation, crystallization,
Dry, obtain thick benzophenone；
2) by step 1) prepare thick benzophenone be placed in rectifying column, be heated to 170-185 DEG C under reduced pressure；
3) step 2) in rectifying column rectifying terminal for rectifying column tower temperature be 220-230 DEG C.
Preferably, described step 1) heating response flow back 4-5 hour, to without hydrogen chloride gas exclude can reaction add
Thermojunction beam.
Preferably, described step 2) in rectifying column tower top pressure be 200-300Pa, temperature be 110-130 DEG C.
Preferably, described step 2) in rectifying column reflux ratio be 3:1.
Preferably, described step 2) in heating temperature be 175-185 DEG C.
Preferably, described step 3) in rectifying terminal for rectifying column tower temperature be 225-230 DEG C.
The invention provides a kind of process for producing of benzophenone, by the way that first benzene is reacted with chlorobenzoyl chloride,
Thick benzophenone is prepared, the difference of different because of raw material sources from production technology is overcome, impurity can be produced, then by essence
Tower distillation operation is evaporated, the high-quality benzophenone of high-purity (purity ＞ 99.89%) can be obtained, while spy controls whole work
The prepared composition of skill, can be further generalized application in actual industrial production.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with implementation of the invention
Example, is clearly and completely described to the technical scheme in the embodiment of the present invention, it is clear that described embodiment is the present invention
A part of embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
The every other embodiment obtained under the premise of creative work is made, the scope of protection of the invention is belonged to.
Embodiment 1：
The present embodiment provides a kind of process for producing of benzophenone, and operating procedure is as follows：
1) dry benzene is added in the retort for being added with chlorobenzoyl chloride, and adds catalyst under agitation
Imported into reaction solution in frozen water and be layered by alchlor, heating reflux reaction, take oil reservoir by drying, decompression, fractionation, crystallization,
Dry, obtain thick benzophenone；
2) by step 1) prepare thick benzophenone be placed in rectifying column, be heated to 170-185 DEG C under reduced pressure；
3) step 2) in rectifying column rectifying terminal for rectifying column tower temperature be 220-230 DEG C.
Step 1) heating response flow back 4-5 hour, to without hydrogen chloride gas exclude can react heating terminate.
Step 2) in rectifying column tower top pressure be 200-300Pa, temperature be 110-130 DEG C.
Step 2) in rectifying column reflux ratio be 3:1.
Embodiment 2：
The present embodiment provides a kind of process for producing of benzophenone, and operating procedure is as follows：
1) dry benzene is added in the retort for being added with chlorobenzoyl chloride, and adds catalyst under agitation
Imported into reaction solution in frozen water and be layered by alchlor, heating reflux reaction, take oil reservoir by drying, decompression, fractionation, crystallization,
Dry, obtain thick benzophenone；
2) by step 1) prepare thick benzophenone be placed in rectifying column, be heated to 175-185 DEG C under reduced pressure；
3) step 2) in rectifying column rectifying terminal for rectifying column tower temperature be 225-230 DEG C.
Step 1) heating response flow back 4-5 hour, to without hydrogen chloride gas exclude can react heating terminate.
Step 2) in rectifying column tower top pressure be 200-300Pa, temperature be 110-130 DEG C.
Step 2) in rectifying column reflux ratio be 3:1.
Embodiment 3：
The present embodiment provides a kind of process for producing of benzophenone, and operating procedure is as follows：
1) dry benzene is added in the retort for being added with chlorobenzoyl chloride, and adds catalyst under agitation
Imported into reaction solution in frozen water and be layered by alchlor, heating reflux reaction, take oil reservoir by drying, decompression, fractionation, crystallization,
Dry, obtain thick benzophenone；
2) by step 1) prepare thick benzophenone be placed in rectifying column, be heated to 170-185 DEG C under reduced pressure；
3) step 2) in rectifying column rectifying terminal for rectifying column tower temperature be 220-230 DEG C.
By first being reacted benzene with chlorobenzoyl chloride, thick benzophenone is prepared, overcome because raw material sources are different
With the difference of production technology, impurity can be produced, then by rectifying column distillation operation, the high-quality hexichol of high-purity can be obtained
Ketone (purity ＞ 99.89%), while spy controls the prepared composition of whole technique, can be further in actual industrial production
Popularization and application.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention has been described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic；And these modification or
Replace, do not make the spirit and scope of the essence disengaging various embodiments of the present invention technical scheme of appropriate technical solution.
Claims (6)
1. a kind of process for producing of benzophenone, it is characterised in that operating procedure is as follows：
1) dry benzene is added in the retort for being added with chlorobenzoyl chloride, and adds catalyst trichlorine under agitation
Change aluminium, imported into reaction solution in frozen water and is layered by heating reflux reaction, take oil reservoir by drying, it is decompression, fractionation, crystallization, dry
It is dry, obtain thick benzophenone；
2) by step 1) prepare thick benzophenone be placed in rectifying column, be heated to 170-185 DEG C under reduced pressure；
3) step 2) in rectifying column rectifying terminal for rectifying column tower temperature be 220-230 DEG C.
2. the process for producing of benzophenone as claimed in claim 1, it is characterised in that described step 1) heating it is anti-
Should flow back 4-5 hours, terminate to heating can be reacted without hydrogen chloride gas exclusion.
3. the process for producing of benzophenone as claimed in claim 1, it is characterised in that described step 2) in rectifying column
The pressure of tower top is 200-300Pa, and temperature is 110-130 DEG C.
4. the process for producing of benzophenone as claimed in claim 1, it is characterised in that described step 2) in rectifying column
Reflux ratio be 3:1.
5. the process for producing of benzophenone as claimed in claim 1, it is characterised in that described step 2) in heating
Temperature is 175-185 DEG C.
6. the process for producing of benzophenone as claimed in claim 1, it is characterised in that described step 3) in rectifying end
Point is 225-230 DEG C for the tower temperature of rectifying column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611127957.8A CN106748691A (en) | 2016-12-09 | 2016-12-09 | The process for producing of benzophenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611127957.8A CN106748691A (en) | 2016-12-09 | 2016-12-09 | The process for producing of benzophenone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106748691A true CN106748691A (en) | 2017-05-31 |
Family
ID=58882028
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611127957.8A Pending CN106748691A (en) | 2016-12-09 | 2016-12-09 | The process for producing of benzophenone |
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| CN (1) | CN106748691A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110872216A (en) * | 2019-12-06 | 2020-03-10 | 南京恒道医药科技有限公司 | Method and device for producing (2-chloro-5-iodophenyl) -4-fluorobenzyl ketone by reaction separation coupling |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030207927A1 (en) * | 2001-12-13 | 2003-11-06 | Wyeth | Phenyl benzisoxazoles as estrogenic agents |
| CN102911028A (en) * | 2011-08-04 | 2013-02-06 | 上海泰禾化工有限公司 | Process for refining benzophenone |
| CN104649880A (en) * | 2013-11-26 | 2015-05-27 | 杨海中 | Method for producing benzophenone |
-
2016
- 2016-12-09 CN CN201611127957.8A patent/CN106748691A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030207927A1 (en) * | 2001-12-13 | 2003-11-06 | Wyeth | Phenyl benzisoxazoles as estrogenic agents |
| CN102911028A (en) * | 2011-08-04 | 2013-02-06 | 上海泰禾化工有限公司 | Process for refining benzophenone |
| CN104649880A (en) * | 2013-11-26 | 2015-05-27 | 杨海中 | Method for producing benzophenone |
Non-Patent Citations (1)
| Title |
|---|
| 薛福连: "紫外线吸收剂二苯甲酮的合成研究", 《精细化工原料及中间体》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110872216A (en) * | 2019-12-06 | 2020-03-10 | 南京恒道医药科技有限公司 | Method and device for producing (2-chloro-5-iodophenyl) -4-fluorobenzyl ketone by reaction separation coupling |
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Application publication date: 20170531 |