CN111875477A - Azeotropic purification method of o-chlorohydrin - Google Patents
Azeotropic purification method of o-chlorohydrin Download PDFInfo
- Publication number
- CN111875477A CN111875477A CN202010769628.3A CN202010769628A CN111875477A CN 111875477 A CN111875477 A CN 111875477A CN 202010769628 A CN202010769628 A CN 202010769628A CN 111875477 A CN111875477 A CN 111875477A
- Authority
- CN
- China
- Prior art keywords
- chlorohydrin
- purification method
- water
- azeotrope
- azeotropic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 11
- 238000000746 purification Methods 0.000 title claims abstract description 11
- 238000004821 distillation Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 5
- 230000020477 pH reduction Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an azeotropic purification method of o-chlorohydrin, the invention only needs the vacuum degree of about-0.080 Mpa to realize normal production, and reduces the distillation temperature, reduces the possibility of over-temperature, effectively prevents corrosive gas, and greatly prolongs the service life of equipment and pipelines; the production period of each batch can be shortened by more than 2-4h, the steam is saved by 1-2 tons, and the energy is saved.
Description
The technical field is as follows:
the invention belongs to the field of chemical industry, and particularly relates to an azeotropic purification method of o-chlorohydrin.
Background art:
the o-chlorohydrin needs to be purified after production, and the existing purification method has high requirements on vacuum degree, namely the vacuum degree of-0.095 Mpa and rectification at the temperature of 128-130 ℃, so that the vacuum pump has high requirements. Under the condition of insufficient vacuum degree, the material is easy to decompose to generate corrosive gas due to over-temperature, so that equipment and pipelines are corroded. And the production cycle is long and the energy consumption is high.
The invention content is as follows:
the invention aims to provide an azeotropic purification method of o-chlorohydrin, the invention can realize normal production only by vacuum degree of about-0.080 Mpa, and reduce distillation temperature, reduce possibility of over-temperature, effectively prevent corrosive gas, and greatly prolong the service life of equipment and pipelines; the production period of each batch can be shortened by more than 2-4h, the steam is saved by 1-2 tons, and the energy is saved.
In order to solve the problems, the technical scheme of the invention is as follows:
an azeotropic purification method of o-chlorohydrin, comprising the following steps:
step one, in the later stage of the o-chloroalcoholic acid acidification distillation, continuously adding water into an o-chloroalcoholic acid acidification reaction kettle at a certain flow rate; water and o-chlorohydrin containing a small amount of light components are subjected to azeotropy to form an azeotrope, and then the azeotrope is heated and rectified to be extracted from the tower top into an intermediate tank; the light fraction is separated off in this way;
step two, standing the azeotrope in an intermediate tank to divide water and obtain an upper oil phase; adding into a rectifying still for circular rectification to obtain the ortho-chlorohydrin.
Further improvement, the temperature of the rectification in the first step is 100-105 ℃; the pressure is-0.075-0.085 MPa.
In a further improvement, the flow rate of the water is 150-200 kg/h.
The invention has the advantages that:
1. normal production can be realized only by vacuum degree of about-0.080 Mpa.
2. The distillation temperature is reduced, the possibility of overtemperature is reduced, corrosive gas is effectively prevented from being generated, and the service lives of equipment and pipelines are greatly prolonged.
3. The production period of each batch can be shortened by more than 2-4h, the steam is saved by 1-2 tons, and the energy is saved.
The specific implementation mode is as follows:
in order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
The invention relates to an o-chlorohydrin azeotropic purification device, which comprises a rectifying tower kettle, a product tank intermediate tank and a circulating pump. The using method of the invention is as follows:
1. continuously adding water into a rectifying tower kettle at a certain flow rate in the later stage of the o-chloroalcoholic acid distillation; water and o-chlorohydrin containing a small amount of light components azeotropy to form an azeotrope, and the azeotrope is extracted from the tower top to an intermediate tank through rectification. In this way the light fraction is separated off.
2. The azeotrope is kept stand in an intermediate tank for water diversion, an upper oil phase (containing a small amount of light component of the ortho-chlorohydrin) is added into a rectifying still for cyclic application, and then the rectified product is input into a product tank.
The above-mentioned embodiment is only a specific embodiment of the present invention, and is not meant to be a limitation of the present invention, and any simple modification and replacement thereof are within the scope of the present invention.
Claims (3)
1. An o-chlorohydrin azeotropic purification method is characterized by comprising the following steps:
step one, in the later stage of the o-chloroalcoholic acid acidification distillation, continuously adding water into an o-chloroalcoholic acid acidification reaction kettle at a certain flow rate; water and o-chlorohydrin containing a small amount of light components are subjected to azeotropy to form an azeotrope, and then the azeotrope is heated and rectified to be extracted from the tower top into an intermediate tank; the light fraction is separated off in this way;
step two, standing the azeotrope in an intermediate tank to divide water and obtain an upper oil phase; adding into a rectifying still for circular rectification to obtain the ortho-chlorohydrin.
2. The azeotropic purification method of o-chlorohydrin as claimed in claim 1, wherein the temperature of the distillation in the first step is 100-105 ℃; the pressure is-0.07 to-0.085 MPa.
3. The azeotropic purification method of o-chlorohydrin as claimed in claim 1, wherein the flow rate of the water is 150-200 kg/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010769628.3A CN111875477A (en) | 2020-08-03 | 2020-08-03 | Azeotropic purification method of o-chlorohydrin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010769628.3A CN111875477A (en) | 2020-08-03 | 2020-08-03 | Azeotropic purification method of o-chlorohydrin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111875477A true CN111875477A (en) | 2020-11-03 |
Family
ID=73206060
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010769628.3A Pending CN111875477A (en) | 2020-08-03 | 2020-08-03 | Azeotropic purification method of o-chlorohydrin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111875477A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58198477A (en) * | 1982-05-12 | 1983-11-18 | Sumitomo Chem Co Ltd | Recovery of epihalohydrin |
| US5227541A (en) * | 1990-07-17 | 1993-07-13 | Showa Denko K.K. | Purification of 2,3-dichloro-1-propanol |
| CN101007751A (en) * | 2007-01-26 | 2007-08-01 | 江苏工业学院 | Preparation method of dichloro propanol from glycerin |
| TW200940489A (en) * | 2005-05-20 | 2009-10-01 | Solvay | Process for producing a chlorohydrin |
| CN101657405A (en) * | 2007-04-12 | 2010-02-24 | 陶氏环球技术公司 | Process and apparatus for azeotropic recovery of dichlorohydrins |
| CN102976897A (en) * | 2012-12-18 | 2013-03-20 | 山东科技大学 | Method for purifying tetrafluoro propanol |
| CN103694082A (en) * | 2013-11-26 | 2014-04-02 | 浙江巨圣氟化学有限公司 | Method for purifying tetrafluoro propanol |
| CN106831339A (en) * | 2016-12-19 | 2017-06-13 | 西安近代化学研究所 | A kind of method for isolating and purifying trifluoroethanol and water azeotropic mixture |
| CN107445799A (en) * | 2016-05-31 | 2017-12-08 | 王圣洁 | Apparatus for producing dichloropropanol and method for producing the same |
-
2020
- 2020-08-03 CN CN202010769628.3A patent/CN111875477A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58198477A (en) * | 1982-05-12 | 1983-11-18 | Sumitomo Chem Co Ltd | Recovery of epihalohydrin |
| US5227541A (en) * | 1990-07-17 | 1993-07-13 | Showa Denko K.K. | Purification of 2,3-dichloro-1-propanol |
| TW200940489A (en) * | 2005-05-20 | 2009-10-01 | Solvay | Process for producing a chlorohydrin |
| CN101007751A (en) * | 2007-01-26 | 2007-08-01 | 江苏工业学院 | Preparation method of dichloro propanol from glycerin |
| CN101657405A (en) * | 2007-04-12 | 2010-02-24 | 陶氏环球技术公司 | Process and apparatus for azeotropic recovery of dichlorohydrins |
| CN102976897A (en) * | 2012-12-18 | 2013-03-20 | 山东科技大学 | Method for purifying tetrafluoro propanol |
| CN103694082A (en) * | 2013-11-26 | 2014-04-02 | 浙江巨圣氟化学有限公司 | Method for purifying tetrafluoro propanol |
| CN107445799A (en) * | 2016-05-31 | 2017-12-08 | 王圣洁 | Apparatus for producing dichloropropanol and method for producing the same |
| CN106831339A (en) * | 2016-12-19 | 2017-06-13 | 西安近代化学研究所 | A kind of method for isolating and purifying trifluoroethanol and water azeotropic mixture |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 414014 Yuehua second industrial zone, Yunxi District, Yueyang City, Hunan Province Applicant after: Yueyang Longxing Industrial Co.,Ltd. Address before: 414014 Yuehua second industrial zone, Yunxi District, Yueyang City, Hunan Province Applicant before: Yueyang Longxing Industrial Co.,Ltd. |
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| CB02 | Change of applicant information | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201103 |
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| RJ01 | Rejection of invention patent application after publication |