CN104844435A - System and technology for producing benzaldehyde by utilizing benzyl chloride and benzyl alcohol waste materials - Google Patents
System and technology for producing benzaldehyde by utilizing benzyl chloride and benzyl alcohol waste materials Download PDFInfo
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- CN104844435A CN104844435A CN201510112100.8A CN201510112100A CN104844435A CN 104844435 A CN104844435 A CN 104844435A CN 201510112100 A CN201510112100 A CN 201510112100A CN 104844435 A CN104844435 A CN 104844435A
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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
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
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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
- C07C45/42—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrolysis
- C07C45/43—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrolysis of >CX2 groups, X being halogen
Abstract
The invention provides a system and a technology for producing benzaldehyde by utilizing benzyl chloride and benzyl alcohol waste materials. The system comprises the main equipment of an oxidizing furnace, an oxidizing kettle, a hydrolyzing kettle, an alkaline hydrolysis kettle, a crude distillation tower, a crude distillation kettle and a rectifying tower. The technological process is simple. The technology solves the discharging problem of the benzyl chloride and benzyl alcohol waste materials, namely dibenzyl ether and benzyl chloride, the waste materials are changed into treasure, and benzaldehyde products with a higher added value are produced. The environmental protection problem is solved, and economic benefits are also created.
Description
Technical field
The present invention relates to phenyl aldehyde production field, particularly relate to a kind of system and the technique that utilize Benzyl Chloride, phenylcarbinol waste material production phenyl aldehyde.
Technical background
The materials at bottom of tower produced after company's Benzyl Chloride product and the rectifying of phenylcarbinol product is mainly benzyl dichloride and dibenzyl ether, and in order to solve the emission problem of these two kinds of waste materials, turn waste into wealth, be raw material production phenyl aldehyde with these two kinds of materials simultaneously.Phenyl aldehyde is a kind of important industrial chemicals, can be used for producing aniline, benzophenone and agrochemical product, is also the most basic raw material of phenyl aldehyde system spices, is the most basic raw material of some pharmaceutical prod of synthesis, plastics additive.
Summary of the invention
The present invention is a kind of technique utilizing the rectifying waste material dibenzyl ether of Benzyl Chloride product and phenylcarbinol product and benzyl dichloride to produce phenyl aldehyde.Dibenzyl ether produces phenyl aldehyde through high-temperature air oxidation.
For solving the problem, the present invention adopts following technical scheme:
Utilize Benzyl Chloride, phenylcarbinol waste material to produce a system for phenyl aldehyde, comprise dibenzyl ether oxidation unit, benzyl dichloride treatment unit, multistage rectification device,
Described dibenzyl ether oxidation unit comprises oxidizing tower, stills for air blowing, slurry tank, crude product storage tank, described oxidizing tower, stills for air blowing, slurry tank, crude product storage tank are connected successively, the top vent of oxidizing tower is connected with air preheater top second inlet mouth, air preheater bottom first row gas port is connected with oxidizing tower bottom air inlet, air preheater bottom second exhaust port is connected with stills for air blowing inlet mouth, and described crude product reservoir outlet is connected with rectifying tower opening for feed;
Benzyl dichloride treatment unit comprises hydrolysis kettle, hydrolysis slurry tank, Hydrolysis of crude tank, alkaline hydrolysis still, alkaline hydrolysis slurry tank, alkaline hydrolysis crude product tank, described hydrolysis kettle, hydrolysis slurry tank, Hydrolysis of crude tank, alkaline hydrolysis still, alkaline hydrolysis slurry tank, alkaline hydrolysis crude product tank are connected successively with thick gold-plating tower, waste liquid relief outlet bottom hydrolysis slurry tank is connected with diluted acid tank fluid inlet, and the waste liquid relief outlet bottom alkaline hydrolysis slurry tank is connected with phenylcarbinol waste water tank fluid inlet;
Described multistage rectification device comprises thick gold-plating tower, thick aldehyde storage tank, rectifying tower, condenser, finished product tundish, described thick gold-plating tower, thick aldehyde storage tank, rectifying tower, condenser, finished product tundish are connected successively, the discharge port of rectifying tower tower top with slightly heat up in a steamer still opening for feed and be connected, slightly heat up in a steamer still air outlet and be connected with thick gold-plating tower bottom inlet mouth.
Further, described air preheater top vent is connected with overhead condenser top inlet mouth.
Further, condenser is provided with between described thick gold-plating tower and thick aldehyde storage tank.
Further, the air outlet at described rectifying tower top is connected with the inlet mouth of crude product storage tank.
Present invention also offers a kind of technique utilizing Benzyl Chloride, phenylcarbinol waste material to produce phenyl aldehyde, comprise the steps:
1) dibenzyl ether is delivered in oxidizing tower, after ascending gas mass-and heat-transfer in stills for air blowing, introduces main stills for air blowing, in main stills for air blowing and oxygen reaction, reaction product is introduced subsider and carry out oily water separation, must be for subsequent use containing the crude product of phenyl aldehyde >=80%;
2) trolamine and benzyl dichloride are joined hydrolysis kettle, utilize low-pressure steam to heat up, in hydrolysis kettle, hydrolysis reaction occurs, collect hydrolyzed solution and lower the temperature through water cooler, after subsider oily water separation, obtain upper strata Hydrolysis of crude and lower floor's dilute acid soln;
3) upper strata Hydrolysis of crude is sent into alkaline hydrolysis still and carry out secondary alkaline hydrolysis, by alkali solution liquid after slurry tank is separated, obtain phenyl aldehyde crude product;
4) by step 1), 3) after the mixing of the phenyl aldehyde crude product that obtains, through slightly heating up in a steamer, rectifying separation and get final product.
Preferably, described oxygen is from pressurized air.
Preferably, mass concentration is adopted to be that the soda ash solution of 10.5%-12% carries out alkali cleaning in described secondary alkaline hydrolysis process.
Beneficial effect of the present invention:
1. the emission problem of the waste material produced after the invention solves Benzyl Chloride product and the rectifying of phenylcarbinol product, utilizes benzyl dichloride and dibenzyl ether to be raw material production phenyl aldehyde.
2. flow process of the present invention is simple, and this technique solves Benzyl Chloride, the waste material dibenzyl ether of phenylcarbinol, the emission problem of benzyl dichloride, and turns waste into wealth, and produces the phenyl aldehyde product that added value is higher.Both solve environmental issue, create economic benefit again.
3. the present invention is with the trolamine aqueous solution as hydrolytic reagent, and do alkaline hydrolysis agent with 10.5%-12% soda ash liquid, the rate of recovery is high, separation is easy, can obtain the phenyl aldehyde product that quality is higher.
Accompanying drawing explanation
Fig. 1 dibenzyl ether oxidation unit schema
Fig. 2 benzyl dichloride treatment unit schema
Fig. 3 multistage rectification device schema
Specific embodiment
Embodiment 1
Utilize Benzyl Chloride, phenylcarbinol waste material to produce the device of phenyl aldehyde, the major equipment comprised is oxidized still, stills for air blowing, hydrolysis kettle, alkaline hydrolysis still, topping still, slightly heat up in a steamer still, rectifying tower.
This technical process is: raw material dibenzyl ether is delivered in oxidizing tower, with the gas mass-and heat-transfer that rises in stills for air blowing, enter main stills for air blowing, phenyl aldehyde is generated with the oxygen reaction in pressurized air in main stills for air blowing, reaction product enters subsider oily water separation, and it is for subsequent use that the obtained crude product containing phenyl aldehyde >=80% enters crude product storage tank.
Hydrolyzed solution and benzyl dichloride join hydrolysis kettle continuously, utilize low-pressure steam to heat up, in hydrolysis kettle, hydrolysis reaction occur.The continuous extraction of hydrolysis reaction liquid, through water cooler cooling, the continuous oily water separation of subsider, lower floor's dilute acid soln is discharged to diluted acid tank bottom subsider, recycles to hydrolyzed solution header tank through pump delivery, and the water that slightly heats up in a steamer slightly heating up in a steamer generation by phenyl aldehyde when hydrolyzed solution lacks supplements.It is for subsequent use that upper strata Hydrolysis of crude is transferred to Hydrolysis of crude tank, then lixiviating solution operation.After secondary alkaline hydrolysis, phenyl aldehyde crude product isolated by lixiviating solution separate and subside tank.The phenyl aldehyde crude product be oxidized with dibenzyl ether mixes through topping still, and the phenyl aldehyde that tower top isolates 95% enters rectifying tower, at rectifying tower side take-off qualified product.
Advantage of the present invention is that flow process is simple, and this technique solves Benzyl Chloride, the waste material dibenzyl ether of phenylcarbinol, the emission problem of benzyl dichloride, and turns waste into wealth, and produces the phenyl aldehyde product that added value is higher.Both solve environmental issue, create economic benefit again.
Embodiment 2
Utilize Benzyl Chloride, phenylcarbinol waste material to produce a system for phenyl aldehyde, comprise dibenzyl ether oxidation unit, benzyl dichloride treatment unit, multistage rectification device,
Described dibenzyl ether oxidation unit comprises oxidizing tower, stills for air blowing, slurry tank, crude product storage tank, described oxidizing tower, stills for air blowing, slurry tank, crude product storage tank are connected successively, the top vent of oxidizing tower is connected with air preheater top second inlet mouth, air preheater bottom first row gas port is connected with oxidizing tower bottom air inlet, air preheater bottom second exhaust port is connected with stills for air blowing inlet mouth, and described crude product reservoir outlet is connected with rectifying tower opening for feed;
Benzyl dichloride treatment unit comprises hydrolysis kettle, hydrolysis slurry tank, Hydrolysis of crude tank, alkaline hydrolysis still, alkaline hydrolysis slurry tank, alkaline hydrolysis crude product tank, described hydrolysis kettle, hydrolysis slurry tank, Hydrolysis of crude tank, alkaline hydrolysis still, alkaline hydrolysis slurry tank, alkaline hydrolysis crude product tank are connected successively with thick gold-plating tower, waste liquid relief outlet bottom hydrolysis slurry tank is connected with diluted acid tank fluid inlet, and the waste liquid relief outlet bottom alkaline hydrolysis slurry tank is connected with phenylcarbinol waste water tank fluid inlet;
Described multistage rectification device comprises thick gold-plating tower, thick aldehyde storage tank, rectifying tower, condenser, finished product tundish, described thick gold-plating tower, thick aldehyde storage tank, rectifying tower, condenser, finished product tundish are connected successively, the discharge port of rectifying tower tower top with slightly heat up in a steamer still opening for feed and be connected, slightly heat up in a steamer still air outlet and be connected with thick gold-plating tower bottom inlet mouth.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (7)
1. utilize Benzyl Chloride, phenylcarbinol waste material to produce a system for phenyl aldehyde, comprise dibenzyl ether oxidation unit, benzyl dichloride treatment unit, multistage rectification device, it is characterized in that,
Described dibenzyl ether oxidation unit comprises oxidizing tower, stills for air blowing, slurry tank, crude product storage tank, described oxidizing tower, stills for air blowing, slurry tank, crude product storage tank are connected successively, the top vent of oxidizing tower is connected with air preheater top second inlet mouth, air preheater bottom first row gas port is connected with oxidizing tower bottom air inlet, air preheater bottom second exhaust port is connected with stills for air blowing inlet mouth, and described crude product reservoir outlet is connected with rectifying tower opening for feed;
Benzyl dichloride treatment unit comprises hydrolysis kettle, hydrolysis slurry tank, Hydrolysis of crude tank, alkaline hydrolysis still, alkaline hydrolysis slurry tank, alkaline hydrolysis crude product tank, described hydrolysis kettle, hydrolysis slurry tank, Hydrolysis of crude tank, alkaline hydrolysis still, alkaline hydrolysis slurry tank, alkaline hydrolysis crude product tank are connected successively with thick gold-plating tower, waste liquid relief outlet bottom hydrolysis slurry tank is connected with diluted acid tank fluid inlet, and the waste liquid relief outlet bottom alkaline hydrolysis slurry tank is connected with phenylcarbinol waste water tank fluid inlet;
Described multistage rectification device comprises thick gold-plating tower, thick aldehyde storage tank, rectifying tower, condenser, finished product tundish, described thick gold-plating tower, thick aldehyde storage tank, rectifying tower, condenser, finished product tundish are connected successively, the discharge port of rectifying tower tower top with slightly heat up in a steamer still opening for feed and be connected, slightly heat up in a steamer still air outlet and be connected with thick gold-plating tower bottom inlet mouth.
2. device as claimed in claim 1, it is characterized in that, described air preheater top vent is connected with overhead condenser top inlet mouth.
3. device as claimed in claim 1, is characterized in that, is provided with condenser between described thick gold-plating tower and thick aldehyde storage tank.
4. device as claimed in claim 1, it is characterized in that, the air outlet at described rectifying tower top is connected with the inlet mouth of crude product storage tank.
5. utilize Benzyl Chloride, phenylcarbinol waste material to produce a technique for phenyl aldehyde, it is characterized in that, comprise the steps:
1) dibenzyl ether is delivered in oxidizing tower, after ascending gas mass-and heat-transfer in stills for air blowing, introduces main stills for air blowing, in main stills for air blowing and oxygen reaction, reaction product is introduced subsider and carry out oily water separation, must be for subsequent use containing the crude product of phenyl aldehyde >=80%;
2) trolamine and benzyl dichloride are joined hydrolysis kettle, utilize low-pressure steam to heat up, in hydrolysis kettle, hydrolysis reaction occurs, collect hydrolyzed solution and lower the temperature through water cooler, after subsider oily water separation, obtain upper strata Hydrolysis of crude and lower floor's dilute acid soln;
3) upper strata Hydrolysis of crude is sent into alkaline hydrolysis still and carry out secondary alkaline hydrolysis, by alkali solution liquid after slurry tank is separated, obtain phenyl aldehyde crude product;
4) by step 1), 3) after the mixing of the phenyl aldehyde crude product that obtains, through slightly heating up in a steamer, rectifying separation and get final product.
6. method described in claim 1, is characterized in that, described oxygen is from pressurized air.
7. method described in claim 1, is characterized in that, adopts mass concentration to be that the soda ash solution of 10.5-12% carries out alkali cleaning in described secondary alkaline hydrolysis process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510112100.8A CN104844435B (en) | 2015-03-16 | 2015-03-16 | A kind of system and technique that benzaldehyde is produced using benzyl chloride, phenmethylol waste material |
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| CN201510112100.8A CN104844435B (en) | 2015-03-16 | 2015-03-16 | A kind of system and technique that benzaldehyde is produced using benzyl chloride, phenmethylol waste material |
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| CN104844435A true CN104844435A (en) | 2015-08-19 |
| CN104844435B CN104844435B (en) | 2018-02-06 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776398A (en) * | 2019-11-08 | 2020-02-11 | 聊城鲁西氯苄化工有限公司 | Benzyl alcohol step pressure hydrolysis reaction process and system |
| CN111517928A (en) * | 2020-04-30 | 2020-08-11 | 武汉有机实业有限公司 | Benzyl ether oxidation process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775285A (en) * | 2012-08-09 | 2012-11-14 | 山东聊城中盛蓝瑞化工有限公司 | Method for producing benzaldehyde by oxidizing dibenzyl ether by air |
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- 2015-03-16 CN CN201510112100.8A patent/CN104844435B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775285A (en) * | 2012-08-09 | 2012-11-14 | 山东聊城中盛蓝瑞化工有限公司 | Method for producing benzaldehyde by oxidizing dibenzyl ether by air |
Non-Patent Citations (2)
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| 天津市染化七厂: "苯甲醛水解工艺改造-以联合水解代替碱性水解获得成功", 《天津化工》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776398A (en) * | 2019-11-08 | 2020-02-11 | 聊城鲁西氯苄化工有限公司 | Benzyl alcohol step pressure hydrolysis reaction process and system |
| CN110776398B (en) * | 2019-11-08 | 2024-03-22 | 鲁西化工集团股份有限公司氯碱化工分公司 | Benzyl alcohol step pressurizing hydrolysis reaction process and system |
| CN111517928A (en) * | 2020-04-30 | 2020-08-11 | 武汉有机实业有限公司 | Benzyl ether oxidation process |
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