CN108395364A - The process for separation and purification of 1,2- dichloropropanes in chloropropene and production of propylene oxide waste liquid - Google Patents
The process for separation and purification of 1,2- dichloropropanes in chloropropene and production of propylene oxide waste liquid Download PDFInfo
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- CN108395364A CN108395364A CN201810398052.7A CN201810398052A CN108395364A CN 108395364 A CN108395364 A CN 108395364A CN 201810398052 A CN201810398052 A CN 201810398052A CN 108395364 A CN108395364 A CN 108395364A
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- propylene oxide
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- chloropropene
- dichloropropanes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- Organic Chemistry (AREA)
- Epoxy Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to industrial waste recycling field, a kind of process for separation and purification of 1,2 dichloropropanes in chloropropene and production of propylene oxide waste liquid is particularly disclosed.The process for separation and purification produces the by-product mother liquor generated during 3 chloropropenes and chlorohydrination production propylene oxide as raw material using high-temperature chlorination, it is characterized in that：After raw material is carried out several grades of washings, through azeotropic distillation, the chloropropyl alcohol in raw material is isolated；The light phase component acquired at the top of rectifying column is condensed and is collected, dichloropropane is refined through three-level washing treatment process；Using process water as extractant, high-purity dichloropropane product is obtained.Step of the present invention is simple, and product purity is high, and equipment is corrosion-free, and operation is continuous, and production efficiency is high, and product quality is stablized, and greatly reduces the discharge capacity of chloropropene and epoxy propane slop, increases the economic benefit of enterprise.
Description
（One）Technical field
The present invention relates to industrial waste recycling field, more particularly to 1,2- in a kind of chloropropene and production of propylene oxide waste liquid
The process for separation and purification of dichloropropane.
（Two）Background technology
During high-temperature chlorination produces chlorallylene and chlorohydrination and produces propylene oxide, the industrial wastes of discharge it is main at
It is divided into 1,2- dichloropropanes.Chlorallylene by-product 1,2- dichloropropanes about 15%；The amount of propylene oxide by-product 1,2- dichloropropanes with
Operating procedure and horizontal different and different, external generally by-product about 15%-18%, advanced country can be down to 10%, the self-built device in China
Some is up to 35%-38%, and causing product, increased production cost.What 1,2- dichloropropanes can be produced as a variety of chemical products
Raw material（Such as agricultural insecticide）, various products can also be transformed by the methods of ammonification, dehydrochlorination, isomerization and chlorinolysis
And intermediate, there is very extensive purposes.Therefore, by-product 1, the higher value application research of 2- dichloropropanes is with very huge
Big market potential.
Before this, domestic propylene oxide by chlorohydrination manufacturer is big absolutely to the dichloropropane byproduct that is generated in production process
Part is burnt up as fuel in input combustion furnace, is used for recovery section heat, is caused the waste significantly of resource.Currently, domestic
Outside to 1,2- dichloropropanes directly using method including preparing novel asphalt coating, Pesticidal composition and as novel dissolvent etc..
Importantly, with 1,2- dichloropropanes are raw material, can be used for preparing important chemical products, including chlorallylene, allyl
The products such as base cyanogen, aryl allyl ether, propylene oxide, propylene, propylene glycol, trichloro ethylene and tetrachloro-ethylene.
At present, although for 1, the Land use systems that there are many 2- dichloropropanes, especially as degreasing solvent and use
In preparing chloropropene, propylene, tetrachloro-ethylene and propylene glycol, promotion prospect is had a vast market.But institute in studying both at home and abroad
1,2- dichloropropane has certain difference with 1, the 2- dichloropropanes in industrial waste, that is, 1,2- in industrial waste
There are many impurity for dichloropropane.Such as 1,2- dichloropropanes in propylene oxide unit waste liquid contain about 15% chloropropyl alcohol, 1%
Water and a small amount of unknown aldehyde, ketone etc..The chloropropyl alcohol contained in 1,2- dichloropropanes not only influences the consumption water of propylene oxide unit
It is flat, no small economic loss is caused, the problems such as 1,2- dichloropropanes poor product quality, color are yellow and smell is big is also resulted in.It is right
The separating-purifying of 1,2- dichloropropanes in waste liquid, which is still, restricts the bottleneck problem that industrial wastes efficiently uses.
（Three）Invention content
In order to compensate for the shortcomings of the prior art, the present invention provides a kind of chloropropenes and epoxy simple for process, product yield is high
Propane produces the process for separation and purification of 1,2- dichloropropanes in waste liquid.
The present invention is achieved through the following technical solutions：
A kind of process for separation and purification of chloropropene and 1,2-Dichloropropane from Waste Liquor in Propylene Oxide Production, is produced with high-temperature chlorination
The by-product mother liquor generated during chlorallylene and chlorohydrination production propylene oxide includes the following steps as raw material：
（1）After raw material is carried out several grades of washings, through azeotropic distillation, rectifying tower pressure interior force is 50-90KPa, tower top temperature 90-
130 DEG C, column bottom temperature is 60-90 DEG C, isolates the chloropropyl alcohol in raw material；
（2）The light phase component acquired at the top of rectifying column is condensed and is collected, dichloropropane is refined through three-level washing treatment process；
（3）Using process water as extractant, high-purity dichloropropane product is obtained.
The present invention, which is examined, is separated chloropropyl alcohol, 2- chloro isopropyl ethers in raw material by washing, azeotropic distillation, azeotropic distillation
Fully consider the parameters such as theoretical cam curve, feed entrance point, reflux ratio and tower top (bottom of tower) produced quantity to by-product mother liquor in the process
The influence of each component separating effect, then by washing, extracting further separating-purifying, obtain high-purity 1,2- dichloropropanes.
The present invention more excellent technical solution be：
Step（1）In, the reflux ratio of rectifying column tower top is 4-12, theoretical cam curve 10-30, steam consumption 100-200kg/
H, cooling water amount 20-50kg/h；Preferably, the reflux ratio of rectifying column tower top be 6-10, theoretical cam curve 15-25,
Steam consumption is 120-160kg/h, cooling water amount 20-30kg/h.
Raw material azeotropic distillation after three-level is washed.
Step（2）In, the condensed device of light phase component is cooled to 30-45 DEG C.
Step（3）In, process water is the process water recycled in chloropropene and propylene oxide production process.
The purity of process using the present invention, 1, the 2- dichloropropanes after separating-purifying reaches 98% or more, water
Divide content control within 50ppm.
Step of the present invention is simple, and product purity is high, and equipment is corrosion-free, and operation is continuous, and production efficiency is high, and product quality is steady
It is fixed, the discharge capacity of chloropropene and epoxy propane slop is greatly reduced, the economic benefit of enterprise is increased.
（Four）Description of the drawings
The present invention will be further described below with reference to the drawings.
Fig. 1 is the process flow diagram of the present invention.
（Five）Specific implementation mode
Embodiment 1：The process for separation and purification of 1,2- dichloropropanes in a kind of chloropropene and production of propylene oxide waste liquid
The by-product mother liquor generated during chlorallylene and chlorohydrination production propylene oxide is produced as original using high-temperature chlorination
Material, includes the following steps：
（1）After raw material is carried out several grades of washings, through azeotropic distillation, rectifying tower pressure interior force is 50KPa, and tower top temperature is 130 DEG C,
Column bottom temperature is 90 DEG C, isolates the chloropropyl alcohol in raw material；
Raw material azeotropic distillation after three-level is washed；The reflux ratio of rectifying column tower top is 12, theoretical cam curve 30, and steam consumption is
200kg/h, cooling water amount 50kg/h；
（2）The condensed device of light phase component acquired at the top of rectifying column is cooled to 45 DEG C of collections, through three-level washing treatment process essence
Dichloropropane processed；
（3）Using process water as extractant, process water is the process water recycled in chloropropene and propylene oxide production process, is obtained
To high-purity dichloropropane product.
Embodiment 2：The process for separation and purification of 1,2- dichloropropanes in a kind of chloropropene and production of propylene oxide waste liquid
The by-product mother liquor generated during chlorallylene and chlorohydrination production propylene oxide is produced as original using high-temperature chlorination
Material, includes the following steps：
（1）After raw material is carried out several grades of washings, through azeotropic distillation, rectifying tower pressure interior force is 90KPa, and tower top temperature is 90 DEG C,
Column bottom temperature is 60 DEG C, isolates the chloropropyl alcohol in raw material；
Raw material azeotropic distillation after three-level is washed；The reflux ratio of rectifying column tower top is 6, theoretical cam curve 10, and steam consumption is
100kg/h, cooling water amount 20kg/h；
（2）The condensed device of light phase component acquired at the top of rectifying column is cooled to 30 DEG C of collections, through three-level washing treatment process essence
Dichloropropane processed；
（3）Using process water as extractant, process water is the process water recycled in chloropropene and propylene oxide production process, is obtained
To high-purity dichloropropane product.
Embodiment 3：The process for separation and purification of 1,2- dichloropropanes in a kind of chloropropene and production of propylene oxide waste liquid
The by-product mother liquor generated during chlorallylene and chlorohydrination production propylene oxide is produced as original using high-temperature chlorination
Material, includes the following steps：
（1）After raw material is carried out several grades of washings, through azeotropic distillation, rectifying tower pressure interior force is 70KPa, and tower top temperature is 100 DEG C,
Column bottom temperature is 70 DEG C, isolates the chloropropyl alcohol in raw material；
Raw material azeotropic distillation after three-level is washed；The reflux ratio of rectifying column tower top is 8, theoretical cam curve 20, and steam consumption is
150kg/h, cooling water amount 30kg/h；
（2）The condensed device of light phase component acquired at the top of rectifying column is cooled to 40 DEG C of collections, through three-level washing treatment process essence
Dichloropropane processed；
（3）Using process water as extractant, process water is the process water recycled in chloropropene and propylene oxide production process, is obtained
To high-purity dichloropropane product.
By high-temperature chlorination produce chlorallylene and chlorohydrination production propylene oxide during generate by-product mother liquor at
Point extremely complex, even more extremely difficult to the Separation ＆ Purification of wherein 1,2- dichloropropanes, component situation is as shown in the table：
The present invention isolates 1,2- dichloropropanes from propylene high-temperature chlorination and propylene oxide by-product, and to 1,2- after separation
Dichloropropane is purified, its content ＞ 98%, moisture ＜ 50ppm are made.
Claims (6)
1. the process for separation and purification of a kind of chloropropene and 1,2-Dichloropropane from Waste Liquor in Propylene Oxide Production, is given birth to high-temperature chlorination
The by-product mother liquor generated during chlorallylene and chlorohydrination production propylene oxide is produced as raw material, it is characterized in that, including such as
Lower step：（1）After raw material is carried out several grades of washings, through azeotropic distillation, rectifying tower pressure interior force is 50-90KPa, and tower top temperature is
90-130 DEG C, column bottom temperature is 60-90 DEG C, isolates the chloropropyl alcohol in raw material；（2）The light phase component that will be acquired at the top of rectifying column
Condensation is collected, and dichloropropane is refined through three-level washing treatment process；（3）Using process water as extractant, high-purity two is obtained
Chloropropane product.
2. the separating-purifying side of 1,2- dichloropropanes in chloropropene according to claim 1 and production of propylene oxide waste liquid
Method, it is characterised in that：Step（1）In, the reflux ratio of rectifying column tower top is 4-12, theoretical cam curve 10-30, and steam consumption is
100-200kg/h, cooling water amount 20-50kg/h.
3. the separating-purifying side of 1,2- dichloropropanes in chloropropene according to claim 1 and production of propylene oxide waste liquid
Method, it is characterised in that：Step（1）In, raw material azeotropic distillation after three-level is washed.
4. the separating-purifying side of 1,2- dichloropropanes in chloropropene according to claim 1 and production of propylene oxide waste liquid
Method, it is characterised in that：Step（2）In, the condensed device of light phase component is cooled to 30-45 DEG C.
5. the analysis purification side of 1,2- dichloropropanes in chloropropene according to claim 1 and production of propylene oxide waste liquid
Method, it is characterised in that：Step（3）In, process water is the process water recycled in chloropropene and propylene oxide production process.
6. the separating-purifying side of 1,2- dichloropropanes in chloropropene according to claim 2 and production of propylene oxide waste liquid
Method, it is characterised in that：The reflux ratio of rectifying column tower top is 6-10, theoretical cam curve 15-25, steam consumption 120-160kg/
H, cooling water amount 20-30kg/h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810398052.7A CN108395364A (en) | 2018-04-28 | 2018-04-28 | The process for separation and purification of 1,2- dichloropropanes in chloropropene and production of propylene oxide waste liquid |
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|---|---|---|---|
| CN201810398052.7A CN108395364A (en) | 2018-04-28 | 2018-04-28 | The process for separation and purification of 1,2- dichloropropanes in chloropropene and production of propylene oxide waste liquid |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1353469A (en) * | 1970-09-23 | 1974-05-15 | Ici Ltd | Propylene dichloride recovery |
| CN104211564A (en) * | 2014-09-16 | 2014-12-17 | 天津大学 | Industrial device and continuous rectification method for extracting 1,2-propylene dichloride from chlorohydrin process epoxypropane waste liquid |
| CN104672051A (en) * | 2013-11-26 | 2015-06-03 | 门修信 | A purification method of 1,2-dichloropropane |
| CN104672052A (en) * | 2015-01-06 | 2015-06-03 | 中国天辰工程有限公司 | Refining method of impure dichloropropane |
-
2018
- 2018-04-28 CN CN201810398052.7A patent/CN108395364A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1353469A (en) * | 1970-09-23 | 1974-05-15 | Ici Ltd | Propylene dichloride recovery |
| CN104672051A (en) * | 2013-11-26 | 2015-06-03 | 门修信 | A purification method of 1,2-dichloropropane |
| CN104211564A (en) * | 2014-09-16 | 2014-12-17 | 天津大学 | Industrial device and continuous rectification method for extracting 1,2-propylene dichloride from chlorohydrin process epoxypropane waste liquid |
| CN104672052A (en) * | 2015-01-06 | 2015-06-03 | 中国天辰工程有限公司 | Refining method of impure dichloropropane |
Non-Patent Citations (2)
| Title |
|---|
| 程能林等: "《溶剂手册上册》", 31 May 1986 * |
| 胡鸿宾: "氯醇法生产环氧丙烷副产物高值化再利用研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
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Application publication date: 20180814 |