CN104211562A - Method for preparing dichloroethane by direct chlorination in presence of composite catalyst - Google Patents
Method for preparing dichloroethane by direct chlorination in presence of composite catalyst Download PDFInfo
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- CN104211562A CN104211562A CN201310206681.2A CN201310206681A CN104211562A CN 104211562 A CN104211562 A CN 104211562A CN 201310206681 A CN201310206681 A CN 201310206681A CN 104211562 A CN104211562 A CN 104211562A
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- composite catalyst
- direct chlorination
- mol ratio
- dichloroethane
- ethene
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a method for preparing dichloroethane by direct chlorination in the presence of a composite catalyst. The method comprises the following steps: introducing ethylene and chlorine gas into a reactor containing a composite catalyst to carry out reactions, and then subjecting the reaction products to the subsequent refining treatments, wherein the composite catalyst is composed of ferric trichloride and NaCl. Through the provided method, the purity of dichloroethane can be increased from 99.6% to 99.7%, and moreover, the preparation method has the advantages of simple operation, economy, practicality, and prominent effect.
Description
Technical field
The present invention relates to the method preparing ethylene dichloride, be specifically related to catalyzer.
Background technology
As everyone knows, ethylene dichloride is the main raw material preparing vinylchlorid.Phase early 1930s, vinylchlorid adopts calcium carbide, and the method for acetylene and hydrogenchloride catalytic addition is produced, and is called for short acetylene method.After, along with the development of petrochemical complex, it is the operational path of raw material that the synthesis of vinylchlorid turns to rapidly with ethene.1940, U.S. combinating carbide company developed dichloroethane law.In order to balance the utilization of chlorine, Japanese Wu Yu chemical industrial company develops again the integrated process by acetylene method and dichloroethane law combination producing vinylchlorid.Nineteen sixty, Dow Chemical company develops the method for ethene through oxychlorination synthesizing chloroethylene, and and dichloroethane law coordinate, being developed to ethene is the complete method of raw material production vinylchlorid, and this method obtains and develops rapidly.Because the requirement of Chemical Manufacture HSE is risen increasingly, the additive methods such as acetylene method, mixing eneyne method are in because energy consumption is high, it is large to pollute the status be progressively eliminated.
1955-1958, the extensive process for oxychlorination of ethylene of chemical company's research of the U.S. is prepared 1,2-ethylene dichloride and is obtained successfully.So far, after, the whole replaced acetylene of ethane becomes the raw material preparing vinylchlorid.To so far, most of factory all adopts ethene direct chlorination (DC) and ethylene oxychlorination (OXY) to prepare 1,2-ethylene dichloride (EDC), then by EDC in addition thermo-cracking obtain vinyl chloride monomer (VCM) combine cut balance DC-EDC-OXY-EDC-VCM method to prepare vinylchlorid.Associating null readings makes full use of cheap raw material, and substantially do not generate by product, the vinylchlorid output of current the Western countries more than 90% is produced by this method.
In process for oxychlorination preparing chloroethylene production technique, high purity prepares the preparation of the method for ethylene dichloride, and namely the rough method for ethylene dichloride is refining, is very important link.
At present, prepare at direct chlorination in the method for the method of ethylene dichloride, chlorine is introduced into coke filter, except the acid mist of deentrainment, then direct chlorination reactor is entered together with ethylene gas, to be dissolved in the iron trichloride (FeCl in ethylene dichloride (EDC)
3) as catalyzer, under 90 DEG C and 0.015MPa, there is addition reaction, generate 1,2-ethylene dichloride (EDC); Direct chlorination reactor is equipped with special gas distributor, and fills the solution of the ferric chloride catalyst of 0.3% (wt).Under present circumstances, the purity of product 1, the 2-ethylene dichloride of this cellular manufacture is about 99.6%, does not first reach the requirement of 99.74% of this unit design, and the secondly too low normal operation that have impact on subsequent cell of product purity, shortens the cycle of operation of subsequent cell.
Summary of the invention
Object of the present invention is providing a kind of method adopting composite catalyst direct chlorination to prepare ethylene dichloride, to overcome the above-mentioned defect that prior art exists.
Method of the present invention, comprise the steps: ethene and chlorine to pass in the reactor being filled with composite catalyst to react, temperature of reaction is 88 ~ 92 DEG C, the mol ratio of ethene and chlorine is 1.2 ~ 1.25, reacted product is sent to follow-up refinement, and described composite catalyst is iron trichloride and NaCl;
In described composite catalyst, Na
+and Fe
3-mol ratio be 0.1 ~ 0.8:1, preferably, Na
+and Fe
3-mol ratio be 0.2 ~ 0.5:1.
The preparation method of described composite catalyst is simple physical mixed.
Adopt method of the present invention, the purity of product ethylene dichloride can rise to 99.7% from 99.6%, and method of the present invention is simple to operate, and economic and practical, successful.
Embodiment
Embodiment 1
Ethene and chlorine are passed in the reactor being filled with composite catalyst and react, temperature of reaction is 88 DEG C, and the mol ratio of ethene and chlorine is 1.2, and reacted product is sent to follow-up refinement; Catalyzer is iron trichloride and NaCl; Na
+and Fe
3-mol ratio be 0.5:1.
Adopt gas chromatography analysis method to carry out analyzing and testing to reaction product, wherein, the purity of product ethylene dichloride is 99.7%.
Embodiment 2
Ethene and chlorine are passed in the reactor being filled with composite catalyst and react, temperature of reaction is 92 DEG C, and the mol ratio of ethene and chlorine is 1.25, and reacted product is sent to follow-up refinement; Catalyzer is iron trichloride and NaCl; Na
+and Fe
3-mol ratio be 0.2:1.
Adopt gas chromatography analysis method to carry out analyzing and testing to reaction product, wherein, the purity of product ethylene dichloride is 99.7%.
Claims (5)
1. adopt composite catalyst direct chlorination to prepare the method for ethylene dichloride, it is characterized in that, comprise the steps: ethene and chlorine to pass in the reactor being filled with catalyzer to react, reacted product is sent to follow-up refinement, and described catalyzer is iron trichloride and NaCl.
2. method according to claim 1, is characterized in that, temperature of reaction is 88 ~ 92 DEG C, and the mol ratio of ethene and chlorine is 1.2 ~ 1.25.
3. method according to claim 1, is characterized in that, in described catalyzer, and Na
+and Fe
3-mol ratio be 0.1 ~ 0.8:1.
4. composite catalyst according to claim 3, is characterized in that, Na
+and Fe
3-mol ratio be 0.2 ~ 0.5:1.
5. method according to claim 2, is characterized in that, described composite catalyst is iron trichloride and NaCl, Na
+and Fe
3-mol ratio be 0.1 ~ 0.8:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310206681.2A CN104211562A (en) | 2013-05-29 | 2013-05-29 | Method for preparing dichloroethane by direct chlorination in presence of composite catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310206681.2A CN104211562A (en) | 2013-05-29 | 2013-05-29 | Method for preparing dichloroethane by direct chlorination in presence of composite catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104211562A true CN104211562A (en) | 2014-12-17 |
Family
ID=52093527
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310206681.2A Pending CN104211562A (en) | 2013-05-29 | 2013-05-29 | Method for preparing dichloroethane by direct chlorination in presence of composite catalyst |
Country Status (1)
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588559A (en) * | 2016-12-14 | 2017-04-26 | 厦门中科易工化学科技有限公司 | Ethylene chlorinating agent for preparing 1,2-dichloroethane, application thereof and preparation method for 1,2-dichloroethane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116846A (en) * | 1993-01-27 | 1996-02-14 | 赫彻斯特股份公司 | Process and device for preparing 1,2-dichlorethane by direct chlorination |
| US6235953B1 (en) * | 1996-07-04 | 2001-05-22 | Vinnolit Monomer Gmbh & Co. Kg | Process for preparing 1,2-dichloroethane by direct chlorination |
-
2013
- 2013-05-29 CN CN201310206681.2A patent/CN104211562A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116846A (en) * | 1993-01-27 | 1996-02-14 | 赫彻斯特股份公司 | Process and device for preparing 1,2-dichlorethane by direct chlorination |
| US6235953B1 (en) * | 1996-07-04 | 2001-05-22 | Vinnolit Monomer Gmbh & Co. Kg | Process for preparing 1,2-dichloroethane by direct chlorination |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106588559A (en) * | 2016-12-14 | 2017-04-26 | 厦门中科易工化学科技有限公司 | Ethylene chlorinating agent for preparing 1,2-dichloroethane, application thereof and preparation method for 1,2-dichloroethane |
| CN106588559B (en) * | 2016-12-14 | 2020-06-05 | 厦门中科易工化学科技有限公司 | Ethylene chlorinating agent for preparing 1, 2-dichloroethane, application thereof and preparation method of 1, 2-dichloroethane |
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Application publication date: 20141217 |