CN101215228A - Tower type continuous dehydration technique for trichloroacetaldehyde monohydrate - Google Patents
Tower type continuous dehydration technique for trichloroacetaldehyde monohydrate Download PDFInfo
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- CN101215228A CN101215228A CNA2007101690790A CN200710169079A CN101215228A CN 101215228 A CN101215228 A CN 101215228A CN A2007101690790 A CNA2007101690790 A CN A2007101690790A CN 200710169079 A CN200710169079 A CN 200710169079A CN 101215228 A CN101215228 A CN 101215228A
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- tower
- chloral hydrate
- dehydration technique
- dewatering
- reaction
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Abstract
Disclosed is a tower type continuous dewatering technology of chloral hydrate, technical characteristic of which is that dilute sulphuric acid is discharged out from the bottom of the tower, the chloral hydrate enters from a certain portion at the bottom of the tower, concentrated sulfuric acid enters from the top of the tower, and refined chloral is discharged out from the top of the tower. The whole process is the continuous dewatering operation and the technique is simple, fast and fluently, which realizes continuous dewatering of chloral hydrate with relatively less equipments and relatively low energy consumption. The technique can be controlled easily and operated relatively stably. Compared with other existing dewatering techniques, the invention not only can reduce investment of equipments, but also is small in area and low in energy consumption. Further, the invention can decrease dewatering cost of chloral hydrate obviously and improve product quality.
Description
Technical field:
The present invention relates to a kind of dewatering of trichoro-aldehyde, the dehydration technique of chloral hydrate serialization specifically method.
Background technology:
Trichoro-aldehyde is the important source material of synthetic SD-1750 of agricultural chemicals and Trichlorphon.Trichoro-aldehyde is that chloral hydrate obtains through vitriol oil dehydration, and China's suitability for industrialized production mostly adopts the semicontinuous dewatering process of still formula at present.The drawback of this technology is that trichoro-aldehyde residence time in still is long, and by the degree height of vitriol oil oxidation, product yield is lower, and material needs through twice vaporization and condensation process the production energy consumption height.Therefore invent a kind of chloral hydrate serialization dehydration technique method, be highly profitable to improve product yield and quality.
Summary of the invention:
Purpose of the present invention is exactly the defective at prior art, and a kind of chloral hydrate serialization dehydration technique method is provided, and it can be made with extra care the chloral hydrate dehydration to high-efficiency and continuous becomes trichoro-aldehyde.
Technical scheme of the present invention is achieved in that it is with dense H in reaction tower
2SO
4Add from cat head, chloral hydrate adds at the bottom of tower, makes H
2SO
4Fully contact the generation dehydration reaction with the chloral hydrate steam in tower, temperature of reaction is 100～120 ℃, and trichoro-aldehyde flows out from cat head.Be that the reaction times is short, side reaction is few, good product quality under 100～120 ℃ the condition in temperature of reaction.
Optimized technical scheme of the present invention is that the control column bottom temperature is 100～150 ℃ in described method; Chloral hydrate and H
2SO
4Weight ratio be 1: 0.5-0.7, described dense H
2SO
4Content be 90～99%.With this understanding, react completely, the reaction times is also short, and trichoro-aldehyde is not easy the oxidation by vitriol oil institute in still.Dense H
2SO
4Content be lower than 90% reaction not exclusively, and speed of response is slow; Dense H
2SO
4Content be higher than 99%, make trichoro-aldehyde oxidized easily.Reaction tower of the present invention is packing tower or tray column.
Chloral hydrate adds the vaporization of tower still continuously and enters at the bottom of the tower, simultaneously, and with the dense H after the preheating
2SO
4Add from cat head, through fully contacting the generation dehydration reaction with the chloral hydrate steam in tower, 100～120 ℃ of temperature of reaction obtain the trichoro-aldehyde of content 〉=98% from cat head.By 100～150 ℃ of temperature at the bottom of the control still, aldehyde contenting amount＜1% at the bottom of the assurance still, sulfuric acid content is 60～80%.
The present invention adopts the serialization dehydration technique, technical process is controlled easily, easy to operate, operate steadily, owing to improved the mass transfer effect of reactant greatly and shortened the residence time of trichoro-aldehyde in dense H2SO4, thereby side reactions such as trichoro-aldehyde high temperature oxidation and decomposition obviously reduced, make the product yield height, quality is good, and energy consumption is low, thereby has reduced production cost.
Embodiment:
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
Trichoro-aldehyde 300g (content 70%) is closed in water intaking, 100 ℃ of control vaporization temperatures, and from the tower still charging of packing tower, 120 ℃ of tower body insulations evenly add dense H from cat head
2SO
4180g, reaction times 15min, overhead collection cut 210g, content 98%, yield are 98%.
Embodiment 2:
Trichoro-aldehyde 300g (content 70%) is closed in water intaking, 150 ℃ of control vaporization temperatures, and from the tower still charging of tray column, 100 ℃ of tower body insulations evenly add dense H from cat head
2SO
4180g, reaction times 10min, overhead collection cut 214g, content 98%, yield are 98.2%.
Embodiment 3:
Trichoro-aldehyde 300g (content 70%) is closed in water intaking, 130 ℃ of control vaporization temperatures, and from the tower still charging of packing tower, 110 ℃ of tower body insulations evenly add dense H from cat head
2SO
4180g, reaction times 20min, overhead collection cut 214g, content 98%, yield are 98.2%.
The simultaneous test of the present invention and the traditional semicontinuous dewatering process of still formula is as follows:
Reaction times temperature of reaction yield
110 ℃ 94% of semicontinuous dewatering process 1 120min of still formula
2 90min 120℃ 94.5％
3 60min 140℃ 94％
120 ℃ 98% of continuousization dehydration technique method 1 10min
2 15min 110℃ 98.2％
3 20min 120℃ 98.2％
Claims (5)
1. chloral hydrate serialization dehydration technique method, it is with dense H in reaction tower
2SO
4Add from cat head, chloral hydrate adds at the bottom of tower, makes H
2SO
4Fully contact the generation dehydration reaction with the chloral hydrate steam in tower, temperature of reaction is 100～120 ℃, and trichoro-aldehyde flows out from cat head.
2. a kind of chloral hydrate serialization dehydration technique method according to claim 1 is characterized in that: the control column bottom temperature is 100～150 ℃ in described method.
3. a kind of chloral hydrate serialization dehydration technique method according to claim 1 and 2 is characterized in that: described dense H
2SO
4Content be 90～98%.
4. a kind of chloral hydrate serialization dehydration technique method according to claim 1 and 2 is characterized in that: chloral hydrate and H
2SO
4Weight ratio be 1: 0.5-0.7.
5. a kind of chloral hydrate serialization dehydration technique method according to claim 1 and 2, it is characterized in that: described reaction tower is packing tower or tray column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101690790A CN101215228A (en) | 2007-12-27 | 2007-12-27 | Tower type continuous dehydration technique for trichloroacetaldehyde monohydrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101690790A CN101215228A (en) | 2007-12-27 | 2007-12-27 | Tower type continuous dehydration technique for trichloroacetaldehyde monohydrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101215228A true CN101215228A (en) | 2008-07-09 |
Family
ID=39621748
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101690790A Pending CN101215228A (en) | 2007-12-27 | 2007-12-27 | Tower type continuous dehydration technique for trichloroacetaldehyde monohydrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101215228A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030623A (en) * | 2010-11-26 | 2011-04-27 | 湘潭大学 | Method for purifying coarse trichloroacetaldehyde |
| CN110922319A (en) * | 2019-10-12 | 2020-03-27 | 湖北省宏源药业科技股份有限公司 | Intermittent distillation-adsorption coupling dehydration technology for chloral hydrate |
-
2007
- 2007-12-27 CN CNA2007101690790A patent/CN101215228A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030623A (en) * | 2010-11-26 | 2011-04-27 | 湘潭大学 | Method for purifying coarse trichloroacetaldehyde |
| CN102030623B (en) * | 2010-11-26 | 2013-02-27 | 湘潭大学 | Method for purifying coarse trichloroacetaldehyde |
| CN110922319A (en) * | 2019-10-12 | 2020-03-27 | 湖北省宏源药业科技股份有限公司 | Intermittent distillation-adsorption coupling dehydration technology for chloral hydrate |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080709 |