CN102453005A - Synthetic method for epoxy chloropropane - Google Patents
Synthetic method for epoxy chloropropane Download PDFInfo
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- CN102453005A CN102453005A CN2010105194630A CN201010519463A CN102453005A CN 102453005 A CN102453005 A CN 102453005A CN 2010105194630 A CN2010105194630 A CN 2010105194630A CN 201010519463 A CN201010519463 A CN 201010519463A CN 102453005 A CN102453005 A CN 102453005A
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- China
- Prior art keywords
- epoxy chloropropane
- reaction
- synthetic method
- temperature
- calcium hydroxide
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- RZTAQXPJZIKSEG-UHFFFAOYSA-N C=[O]C(CN)CN Chemical compound C=[O]C(CN)CN RZTAQXPJZIKSEG-UHFFFAOYSA-N 0.000 description 1
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- Epoxy Compounds (AREA)
Abstract
The invention discloses a synthetic method for epoxy chloropropane, which belongs to the technical field of petrochemical industry, and particularly relates to a synthetic method for epoxy chloropropane. The invention provides a synthetic method for epoxy chloropropane, which has low time consumption and high yield. The method comprises the following synthetic steps of: putting a three-neck flask into an oil bath boiler; adding dichlorohydrin and calcium hydroxide into the flask in the molar ratio of 1:1-1.3:1 for undergoing a cyclization reaction at the temperature of 40-70 DEG C for 20-50 minutes; neutralizing a reaction product with hydrochloric acid, and stripping and distilling with water vapor; controlling the temperature at 90 DEG C; condensing mixed vapor and laminating; drying a subnatant with anhydrous calcium chloride and standing over night; and distilling and collecting fractions of 80-82 DEG C/33,000 Pa under reduced pressure.
Description
Technical field:
The invention belongs to the petrochemical technology field, in particular, relate to a kind of compound method of epoxy chloropropane.
Background technology:
Non-renewable and the price of petroleum resources high rapidly forces people to seek its substitute, and utilizing natural fats and oils to replace petroleum product becomes focus.Natural fats and oils has recyclability, can make biofuel and tensio-active agent, meets tensio-active agent greenization development trend.The biological diesel oil byproduct glycerin deep processing is for promoting biofuel and green surfactant industry that important meaning is arranged, and that wherein have most the industrialization development prospect is glycerine system epoxy chloropropane (ECH).
Epoxy chloropropane has another name called Epicholorohydrin, and molecular formula is C
3H
5ClO is for volatility is high, unsettled liquid.It is a main raw material of producing epoxy resin, chlorohydrin rubber etc., also can produce tensio-active agent and other fine chemicals simultaneously.The working method of ECH mainly contains two big types: be raw material and be raw material with the by-product glycerin of renewable grease processing with non-renewable petroleum resources.Though these two types of working methods all have midbody dichlorohydrine (DCH) to generate, because of the composition content of two kinds of isomer among the different DCH of operational path has very big difference.Two kinds of equal long reaction times of method, yield are low.
Summary of the invention:
The present invention is exactly to the problems referred to above, and the compound method of a kind of weak point consuming time, epoxy chloropropane that yield is high is provided.
In order to realize above-mentioned purpose of the present invention, synthesis step of the present invention is: there-necked flask is put into oil bath pan, and adding dichlorohydrine and calcium hydroxide carry out cyclization in flask; The mol ratio of calcium hydroxide and dichlorohydrine is 1: 1～1: 1.3; Temperature is controlled at 40～70 ℃, reaction 20～50min, and reaction product neutralizes with hydrochloric acid after the distillation of water vapour stripping; Control 90 ℃; The Calcium Chloride Powder Anhydrous dried overnight is used in layering after the mixing steam condensation, subnatant, and 80～82 ℃/33000Pa cut is collected in underpressure distillation.
Reaction equation is:
Beneficial effect of the present invention:
1. the present invention's weak point consuming time, environmental pollution is little;
2. yield of the present invention is 93.1%.
Embodiment:
Synthesis step of the present invention is: there-necked flask is put into oil bath pan, and adding dichlorohydrine and calcium hydroxide carry out cyclization in flask, and the mol ratio of calcium hydroxide and dichlorohydrine is 1: 1～1: 1.3; Temperature is controlled at 40～70 ℃, reaction 20～50s, and reaction product neutralizes with hydrochloric acid after the distillation of water vapour stripping; Control 90 ℃; The Calcium Chloride Powder Anhydrous dried overnight is used in layering after the mixing steam condensation, subnatant, and 80～82 ℃/33000Pa cut is collected in underpressure distillation.
Reaction equation is:
Product structure of the present invention has obtained the affirmation of nuclear magnetic spectrogram and mass spectrum.
The present invention selects mol ratio, temperature of reaction, reaction times as the factor that influences product yield, visible table 1.A is the mol ratio of calcium hydroxide and dichlorohydrine in the table 1, B be temperature of reaction (℃), C is reaction times (s).
Table 1 three factors are to the influence of yield
| Sequence number | A | B | C | Yield/% |
| 1 | 1.0∶1.0 | 40 | 20 | 84.0 |
| 2 | 1.0∶1.0 | 50 | 30 | 87.7 |
| 3 | 1.0∶1.0 | 60 | 40 | 87.8 |
| 4 | 1.0∶1.0 | 70 | 50 | 84.5 |
| 5 | 1.1∶1.0 | 40 | 30 | 88.6 |
| 6 | 1.1∶1.0 | 50 | 20 | 89.4 |
| 7 | 1.1∶1.0 | 60 | 50 | 88.3 |
| 8 | 1.1∶1.0 | 70 | 40 | 86.0 |
| 9 | 1.2∶1.0 | 40 | 40 | 89.0 |
| 10 | 1.2∶1.0 | 50 | 50 | 92.7 |
| 11 | 1.2∶1.0 | 60 | 20 | 91.9 |
| 12 | 1.2∶1.0 | 70 | 30 | 89.1 |
| 13 | 1.3∶1.0 | 40 | 50 | 86.2 |
| 14 | 1.3∶1.0 | 50 | 40 | 89.5 |
| 15 | 1.3∶1.0 | 60 | 30 | 88.1 |
| 16 | 1.3∶1.0 | 70 | 20 | 86.8 |
As a kind of preferred version, synthesis step of the present invention is: the mol ratio of calcium hydroxide and dichlorohydrine is 1.2: 1.0, and temperature of reaction is 50 ℃, and the reaction times is 20s.
Claims (2)
1. the compound method of an epoxy chloropropane is characterized in that, synthesis step of the present invention is: there-necked flask is put into oil bath pan; Adding dichlorohydrine and calcium hydroxide carry out cyclization in flask, and the mol ratio of calcium hydroxide and dichlorohydrine is 1: 1～1: 1.3, and temperature is controlled at 40～70 ℃; Reaction 20～50min; Reaction product after the water vapour stripping distills, is controlled 90 ℃, layering after the mixing steam condensation with the hydrochloric acid neutralization; Subnatant is used the Calcium Chloride Powder Anhydrous dried overnight, and 80～82 ℃/33000Pa cut is collected in underpressure distillation.
2. the compound method of a kind of epoxy chloropropane according to claim 1 is characterized in that, synthesis step of the present invention is: the mol ratio of calcium hydroxide and dichlorohydrine is 1.2: 1.0, and temperature of reaction is 50 ℃, and the reaction times is 20s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105194630A CN102453005A (en) | 2010-10-25 | 2010-10-25 | Synthetic method for epoxy chloropropane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105194630A CN102453005A (en) | 2010-10-25 | 2010-10-25 | Synthetic method for epoxy chloropropane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102453005A true CN102453005A (en) | 2012-05-16 |
Family
ID=46036733
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105194630A Pending CN102453005A (en) | 2010-10-25 | 2010-10-25 | Synthetic method for epoxy chloropropane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102453005A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012321A (en) * | 2012-12-12 | 2013-04-03 | 常州大学 | Method and system thereof for synthesizing epoxy chloropropane by dichloropropanol |
| CN107973760A (en) * | 2017-10-13 | 2018-05-01 | 江苏索普（集团）有限公司 | The method for preparing epoxychloropropane |
-
2010
- 2010-10-25 CN CN2010105194630A patent/CN102453005A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012321A (en) * | 2012-12-12 | 2013-04-03 | 常州大学 | Method and system thereof for synthesizing epoxy chloropropane by dichloropropanol |
| CN103012321B (en) * | 2012-12-12 | 2015-04-15 | 常州大学 | Method and system thereof for synthesizing epoxy chloropropane by dichloropropanol |
| CN107973760A (en) * | 2017-10-13 | 2018-05-01 | 江苏索普（集团）有限公司 | The method for preparing epoxychloropropane |
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| DD01 | Delivery of document by public notice |
Addressee: Ma Zi Document name: Notification of Passing Preliminary Examination of the Application for Invention |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120516 |