CN102584519A - Preparation method of chloroisoamylene - Google Patents
Preparation method of chloroisoamylene Download PDFInfo
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- CN102584519A CN102584519A CN2012100130415A CN201210013041A CN102584519A CN 102584519 A CN102584519 A CN 102584519A CN 2012100130415 A CN2012100130415 A CN 2012100130415A CN 201210013041 A CN201210013041 A CN 201210013041A CN 102584519 A CN102584519 A CN 102584519A
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- isoprene
- chloroisoamylene
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- hydrogen chloride
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Abstract
The invention discloses a preparation method of chloroisoamylene, belonging to the technical field of chemical industry. The method comprises the following steps of: preparing isoprene and chlorine hydride serving as raw materials; adding copper acetate serving as a catalyst into the isoprene serving as a raw material; stirring uniformly; introducing chlorine hydride gas into a mixture for reacting; stopping introducing chlorine hydride gas when the content of isoprene in the reaction mixture is 1-8 percent according to gas chromatographic analysis; stopping reacting; stirring for 3-5 hours; standing for 2-3 hours; and putting a reaction material into a storage tank. According to the method, the reaction rate and product yield of chloroisoamylene are increased effectively, and the product yield can be over 88 percent.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of preparation method of chloroisoamylene.
Background technology
Chloroisoamylene is a kind of important chemical intermediate feed, is used for synthetic perfume, makes foodstuff additive, pharmaceutical prod etc.
Chloroisoamylene can be made through addition reaction by hydrogen chloride gas and isoprene.The addition reaction of hydrogenchloride and isoprene generates 1-chloroisoamylene and 3-chloroisoamylene simultaneously, and reaction formula is following:
Usually the addition reaction hydrogen chloride gas is excessive adding, and this addition reaction is thermopositive reaction, and under the temperature condition with higher, the 3-chloroisoamylene is prone to generate by product 2-chloro iso-pentane with the further addition of hydrogenchloride, and reaction formula is following:
This side reaction meeting obviously reduces the yield of chloroisoamylene, in order to improve the yield of chloroisoamylene, reduces by product 2-chloro iso-pentane; At present domestic producers use cuprous chloride as catalyzer; Improve the yield of chloroisoamylene, reduce the generation of by product 2-chloro iso-pentane, but because the solvability of this catalyzer of cuprous chloride is lower; Cuprous chloride is difficult to be dissolved in and carries out catalysis in the reactant; Thereby cause speed of reaction slow, the yield of product chloroisoamylene is also not satisfactory simultaneously, generally about 85%.
Summary of the invention
The invention provides a kind of preparation method of chloroisoamylene, slow to solve among the existing chloroisoamylene preparation method speed of reaction, the problem that product yield is low.
The concrete technical scheme that the present invention solves the problems of the technologies described above is:
A kind of compound method of chloroisoamylene is provided, and this method is a raw material with isoprene and hydrogenchloride, and its characteristic may further comprise the steps:
1) uses neutralized verdigris as catalyzer, join in the raw material isoprene, and stir;
2) in said mixture, feed hydrogen chloride gas and react, according to gas chromatographic analysis, when the isoprene content in the reaction mixture is in 1-8%, stop to feed hydrogen chloride gas, reaction finishes;
3) stir 3-5 hour then, left standstill again 2-3 hour, reaction mass is put into storage tank, set aside for use.
To account for the mass percent of isoprene be 0.2-0.3% to catalyst acetic acid copper in the above-mentioned compound method.
Key of the present invention is to be between the 1-8% through the isoprene content in the gas chromatographic analysis control reaction product; Use the neutralized verdigris catalyzer to substitute cuprous chloride catalyst of the prior art simultaneously.
Adopt technical scheme of the present invention, the positively effect of generation is:
1, is between the 1-8% through the isoprene content in the gas chromatographic analysis control reaction product; Thereby guarantee the inexcessive adding of raw material hydrogen chloride gas; Prevent that effectively the 3-chloroisoamylene in the reaction product from continuing to generate by product 2-chloro iso-pentane with hcl reaction, thereby improved the reaction yield of chloroisoamylene.
2, replace cuprous chloride with neutralized verdigris, it is low to have overcome former reaction time catalizer solvability, the shortcoming that speed of reaction is slow, and the solvability of neutralized verdigris catalyzer is high, can dissolve each other preferably with isoprene, improves speed of reaction, and then has improved product yield.
Technical scheme of the present invention can make the reaction yield of chloroisoamylene bring up to more than 88%, has obtained good economic benefit.
Embodiment
The embodiment of the invention has adopted the neutralized verdigris catalyzer of different mass per-cent, through controlling isoprene content in the different products, is exemplified below respectively.
Embodiment 1
1, nitrogen replacement: feed nitrogen at synthesis reactor and replace twice;
2, add isoprene: open the charging valve, open nitrogen valve goalkeeper 2000kg isoprene and be pressed in the synthesis reactor;
3, add catalyzer: in synthesis reactor, add the neutralized verdigris of 5kg, and stir;
4, cooling: open the cooling valve, make the synthesis reactor temperature reduce to 5-10 ℃;
5, reaction: feed hydrogen chloride gas, according to the analysis of gc, when the content of isoprene reaches 5%, stop to feed hydrogen chloride gas, reaction finishes;
6, store: close logical nitrogen valve, under 10 ℃ of temperature, stirred 4 hours, static 2.5 hours, reaction mass is put into the chloroisoamylene storage tank through taking out batch can, set aside for use obtains the about 2904kg of chloroisoamylene, yield about 91.7%.
Embodiment 2
1, nitrogen replacement: feed nitrogen at synthesis reactor and replace twice;
2, add isoprene: open the charging valve, open nitrogen valve goalkeeper 2000kg isoprene and be pressed in the synthesis reactor;
3, add catalyzer: in synthesis reactor, add the neutralized verdigris of 6kg, and stir;
4, cooling: open the cooling valve, make the synthesis reactor temperature reduce to 5-10 ℃;
5, reaction: feed hydrogen chloride gas, according to the analysis of gc, when the content of isoprene reaches 1%, stop to feed hydrogen chloride gas, reaction finishes;
6, store: close logical nitrogen valve, under 10 ℃ of temperature, stirred 4 hours, static 2.5 hours, reaction mass is put into the chloroisoamylene storage tank through taking out batch can, set aside for use obtains the about 2928kg of chloroisoamylene, yield about 87.6%.
Embodiment 3
1, nitrogen replacement: feed nitrogen at synthesis reactor and replace twice;
2, add isoprene: open the charging valve, open nitrogen valve goalkeeper 2000kg isoprene and be pressed in the synthesis reactor;
3, add catalyzer: in synthesis reactor, add the neutralized verdigris of 4kg, and stir;
4, cooling: open the cooling valve, make the synthesis reactor temperature reduce to 5-10 ℃;
5, reaction: feed hydrogen chloride gas, according to the analysis of gc, when the content of isoprene reaches 8%, stop to feed hydrogen chloride gas, reaction finishes;
6, store: close logical nitrogen valve, under 10 ℃ of temperature, stirred 4 hours, static 2.5 hours, reaction mass is put into the chloroisoamylene storage tank through taking out batch can, set aside for use obtains the about 2870kg of chloroisoamylene, yield about 88.2%.
Claims (2)
1. the preparation method of a chloroisoamylene, this method is a raw material with isoprene and hydrogenchloride, its characteristic may further comprise the steps:
1) uses neutralized verdigris as catalyzer, join in the raw material isoprene, and stir;
2) in said mixture, feed hydrogen chloride gas and react, according to gas chromatographic analysis, when the isoprene content in the reaction mixture is in 1-8%, stop to feed hydrogen chloride gas, reaction finishes;
3) stir 3-5 hour then, left standstill again 2-3 hour, reaction mass is put into storage tank, set aside for use.
2. the preparation method of a kind of chloroisoamylene according to claim 1, it is characterized in that: the mass percent that said catalyst acetic acid copper accounts for isoprene is 0.2-0.3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012100130415A CN102584519A (en) | 2012-01-17 | 2012-01-17 | Preparation method of chloroisoamylene |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100130415A CN102584519A (en) | 2012-01-17 | 2012-01-17 | Preparation method of chloroisoamylene |
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| CN102584519A true CN102584519A (en) | 2012-07-18 |
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| CN2012100130415A Pending CN102584519A (en) | 2012-01-17 | 2012-01-17 | Preparation method of chloroisoamylene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924224A (en) * | 2012-11-02 | 2013-02-13 | 南通天泽化工有限公司 | Preparation technique of 1-chloro-3-methyl-2-butene |
| CN105523882A (en) * | 2015-12-16 | 2016-04-27 | 绍兴明业化纤有限公司 | Method for inhibiting explosive polymerization of chloroisopentene and device thereof |
| CN109180450A (en) * | 2018-10-09 | 2019-01-11 | 南通天泽化工有限公司 | A kind of preparation method of methyl heptenone |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU480691A1 (en) * | 1974-03-20 | 1975-08-15 | Калужский филиал Всесоюзного научно-исследовательского института синтетических и натуральных душистых веществ | The method of producing monohydrochloride isoprene |
| CN102126918A (en) * | 2010-12-16 | 2011-07-20 | 江苏优士化学有限公司 | Method for preparing 1-chloroisoamylene |
-
2012
- 2012-01-17 CN CN2012100130415A patent/CN102584519A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU480691A1 (en) * | 1974-03-20 | 1975-08-15 | Калужский филиал Всесоюзного научно-исследовательского института синтетических и натуральных душистых веществ | The method of producing monohydrochloride isoprene |
| CN102126918A (en) * | 2010-12-16 | 2011-07-20 | 江苏优士化学有限公司 | Method for preparing 1-chloroisoamylene |
Non-Patent Citations (1)
| Title |
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| 邵锡宸: "氯代异戊烯的异构化及其与分馏装置材料的关系", 《化学世界》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924224A (en) * | 2012-11-02 | 2013-02-13 | 南通天泽化工有限公司 | Preparation technique of 1-chloro-3-methyl-2-butene |
| CN102924224B (en) * | 2012-11-02 | 2014-12-03 | 南通天泽化工有限公司 | Preparation technique of 1-chloro-3-methyl-2-butene |
| CN105523882A (en) * | 2015-12-16 | 2016-04-27 | 绍兴明业化纤有限公司 | Method for inhibiting explosive polymerization of chloroisopentene and device thereof |
| CN109180450A (en) * | 2018-10-09 | 2019-01-11 | 南通天泽化工有限公司 | A kind of preparation method of methyl heptenone |
| CN109180450B (en) * | 2018-10-09 | 2021-12-28 | 南通天泽化工有限公司 | Preparation method of methyl heptenone |
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Application publication date: 20120718 |