CN101704707B - Method for removing impurity from trichloropropane - Google Patents
Method for removing impurity from trichloropropane Download PDFInfo
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- CN101704707B CN101704707B CN 200910050076 CN200910050076A CN101704707B CN 101704707 B CN101704707 B CN 101704707B CN 200910050076 CN200910050076 CN 200910050076 CN 200910050076 A CN200910050076 A CN 200910050076A CN 101704707 B CN101704707 B CN 101704707B
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- trichloropropane
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Abstract
The invention relates to a method for removing an impurity from trichloropropane, which comprises the following steps: adding trichloro ethane containing a dichloropropanol impurity into a reaction kettle with a stirring device; adding hydrochloric acid and chloridizing reagent into reaction liquid; keeping the reaction temperature at 70 to 90 DEG C and performing reaction with stirring; taking a sample to analyze and detect if all dichloropropanol in the sample is converted into trichloropropane; if all dichloropropanol in the sample is converted into trichloropropane, stopping reaction; and then subjecting the reaction solution into distillation at reduced pressure to obtain trichloropropane and raffinate containing the chloridizing reagent at the same time. Compared with the prior art, the method has the advantages that: the dichloropropanol impurity is converted into the trichloropropane, so high-purity trichloropropane can be obtained and the production cost is reduced; and the distillation at reduced pressure is adopted in production, so the production operation is more convenient.
Description
Technical field
The present invention relates to a kind of removal method of impurity, especially relate to the removal method of impurity in a kind of trichloropropane.
Background technology
At present; Need use trichloropropane as raw material when producing dichloropropylene; But in order to reduce cost; Enterprise often adopts the trichloropropane that contains the impurity dichlorohydrine as raw material, but when adopting this trichloropropane that contains the impurity dichlorohydrine as raw material, carries out next step reaction and can produce a large amount of impurity and have a strong impact on the finished product yield.Present most of producer all adopts the method for rectifying to separate; But the boiling point of trichloropropane is 157 ℃ under the normal pressure, and the boiling point of dichlorohydrine is 175 ℃; Both boiling points are very close; Cause when actually operating and can only the rectifying tower reflux ratio be transferred greatly, cause energy consumption higher, and actual separating effect is relatively poor.
Summary of the invention
The object of the invention is exactly that a kind of removal method that can obtain impurity in the lower trichloropropane of highly purified trichloropropane, production cost is provided in order to overcome the defective that above-mentioned prior art exists.
The object of the invention can be realized through following technical scheme:
The removal method of impurity is characterized in that in a kind of trichloropropane, and this method may further comprise the steps: the trichloroethane that will contain massfraction and be the 20-30% dichlorohydrine joins in the reaction kettle that has whipping appts; In this reaction solution, adding concentration expressed in percentage by weight is the hydrochloric acid of 30-35%, adds chlorination reagent again, and control reaction temperature is at 70-90 ℃; Stirring reaction; The sampling carry out analyzing and testing wherein dichlorohydrine all be converted into trichloropropane, stopped reaction carries out underpressure distillation with reaction soln afterwards; Promptly obtain trichloropropane, the remaining raffinate that contains chlorination reagent is applied mechanically to following batch and is used as catalyzer in the reaction kettle.
The weight ratio of described trichloroethane, hydrochloric acid and chlorination reagent is 1: (0.16-0.2): (0.12-0.16).
Described chlorination reagent comprises zinc chloride, phosphorus trichloride, phosphorus pentachloride, sulfur oxychloride or aluminum chloride.
The preferred zinc chloride of described chlorination reagent.
Compared with prior art, the present invention is a trichloropropane with the chlorination of impurity dichlorohydrine, helps obtaining highly purified trichloropropane and reduces production costs.The trichloropropane that contains the impurity dichlorohydrine for processing has good effect, can adopt underpressure distillation aborning, greatly facilitates production operation.
Embodiment
Embodiment below in conjunction with embodiment is done further to specify to foregoing of the present invention again, but should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following instance.Do not breaking away under the above-mentioned technological thought situation of the present invention, various replacements or change according to ordinary skill knowledge and customary means are made all should comprise within the scope of the invention.
Embodiment 1
The trichloroethane that 500g is contained 20% impurity dichlorohydrine joins in the reaction kettle that has whipping appts, and the adding concentration expressed in percentage by weight is 30% hydrochloric acid 80g in this reaction solution, adds zinc chloride 60g again; Control reaction temperature is at 70 ℃, stirring reaction, sampling carry out analyzing and testing wherein dichlorohydrine all be converted into trichloropropane; Stopped reaction; Afterwards reaction soln is carried out underpressure distillation, promptly obtain the qualified trichloropropane product of 480g, can also obtain the raffinate that 80g contains zinc chloride simultaneously.
Embodiment 2
The trichloroethane that 500g is contained 25% impurity dichlorohydrine joins in the reaction kettle that has whipping appts, and the adding concentration expressed in percentage by weight is 32% hydrochloric acid 90g in this reaction solution, adds aluminum chloride 70g again; Control reaction temperature is at 80 ℃, stirring reaction, sampling carry out analyzing and testing wherein dichlorohydrine all be converted into trichloropropane; Stopped reaction; Afterwards reaction soln is carried out underpressure distillation, promptly obtain the qualified trichloropropane product of 485g, can also obtain the raffinate that 85g contains aluminum chloride simultaneously.
Embodiment 3
The trichloroethane that 500g is contained 28% impurity dichlorohydrine joins in the reaction kettle that has whipping appts; The adding concentration expressed in percentage by weight is 30% hydrochloric acid 90g in this reaction solution, adds the raffinate 80g that obtains containing zinc chloride among the embodiment 1 again, and control reaction temperature is at 80 ℃; Stirring reaction; The sampling carry out analyzing and testing wherein dichlorohydrine all be converted into trichloropropane, stopped reaction carries out underpressure distillation with reaction soln afterwards; Promptly obtain the qualified trichloropropane product of 475g, can also obtain the raffinate that 80g contains zinc chloride simultaneously.
Embodiment 4
The trichloroethane that 500g is contained 30% impurity dichlorohydrine joins in the reaction kettle that has whipping appts; The adding concentration expressed in percentage by weight is 35% hydrochloric acid 100g in this reaction solution, adds the raffinate 80g that obtains containing aluminum chloride among the embodiment 2 again, and control reaction temperature is at 80 ℃; Stirring reaction; The sampling carry out analyzing and testing wherein dichlorohydrine all be converted into trichloropropane, stopped reaction carries out underpressure distillation with reaction soln afterwards; Promptly obtain the qualified trichloropropane product of 482g, can also obtain the raffinate that 81g contains aluminum chloride simultaneously.
Claims (3)
1. the removal method of impurity in the trichloropropane is characterized in that this method may further comprise the steps: the trichloropropane that will contain massfraction and be the 20-30% dichlorohydrine joins in the reaction kettle that has whipping appts; In this solution, adding concentration expressed in percentage by weight is the hydrochloric acid of 30-35%; Add chlorination reagent again, control reaction temperature is at 70-90 ℃, the stirring reaction sampling carry out analyzing and testing wherein dichlorohydrine all be converted into trichloropropane; Stopped reaction; Afterwards reaction soln is carried out underpressure distillation, promptly obtain trichloropropane, the remaining raffinate that contains chlorination reagent is applied mechanically to following batch and is used as catalyzer in the reaction kettle;
Described chlorination reagent is zinc chloride or aluminum chloride.
2. the removal method of impurity is characterized in that in a kind of trichloropropane according to claim 1, and the weight ratio of described trichloropropane, hydrochloric acid and chlorination reagent is 1: (0.16-0.2): (0.12-0.16).
3. the removal method of impurity is characterized in that in a kind of trichloropropane according to claim 1, the preferred aluminum chloride of described chlorination reagent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910050076 CN101704707B (en) | 2009-04-27 | 2009-04-27 | Method for removing impurity from trichloropropane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910050076 CN101704707B (en) | 2009-04-27 | 2009-04-27 | Method for removing impurity from trichloropropane |
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| Publication Number | Publication Date |
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| CN101704707A CN101704707A (en) | 2010-05-12 |
| CN101704707B true CN101704707B (en) | 2012-12-19 |
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| CN 200910050076 Active CN101704707B (en) | 2009-04-27 | 2009-04-27 | Method for removing impurity from trichloropropane |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044187B (en) * | 2013-01-17 | 2015-07-29 | 江苏银珠化工集团有限公司 | A kind of method and system of producing monochloroethane |
| CN106336341B (en) * | 2016-08-22 | 2018-08-21 | 中南林业科技大学 | A kind of technique of synthesis chloroethanes |
| CN107602341A (en) * | 2017-10-18 | 2018-01-19 | 王佳琦 | A kind of method from epoxy height boiling extraction trichloropropane |
| CN110068621A (en) * | 2018-01-23 | 2019-07-30 | 苏州电器科学研究院股份有限公司 | A kind of detection method effectively measuring 1,2,3- trichloropropane contents in electronic material |
| CN109678647A (en) * | 2018-08-22 | 2019-04-26 | 浙江万盛股份有限公司 | A kind of preparation method of high-purity 1- chlorine normal butane |
| CN111018665A (en) * | 2019-12-17 | 2020-04-17 | 山东民基化工有限公司 | Method for recycling trichloropropane in epichlorohydrin heavy component |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053422A (en) * | 1991-02-05 | 1991-07-31 | 齐鲁石油化工公司研究院 | From the by-product fluorocarbon oil, extract the method for alkyl chloride |
| CN1275558A (en) * | 1999-05-26 | 2000-12-06 | 中国石化集团齐鲁石油化工公司 | Extraction separating method for dichloropropand |
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2009
- 2009-04-27 CN CN 200910050076 patent/CN101704707B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053422A (en) * | 1991-02-05 | 1991-07-31 | 齐鲁石油化工公司研究院 | From the by-product fluorocarbon oil, extract the method for alkyl chloride |
| CN1275558A (en) * | 1999-05-26 | 2000-12-06 | 中国石化集团齐鲁石油化工公司 | Extraction separating method for dichloropropand |
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| CN101704707A (en) | 2010-05-12 |
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Address after: 226407 chemical industry zone, Rudong County, Jiangsu Province Patentee after: Nantong Taihe chemical Limited by Share Ltd Address before: 226407, Rudong County, Jiangsu Province mouth chemical industry park Patentee before: Nantong Taihe Chemical Co., Ltd. |