CN105732320A - Purifying method for 1,4-cyclohexanedimethanol - Google Patents
Purifying method for 1,4-cyclohexanedimethanol Download PDFInfo
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- CN105732320A CN105732320A CN201610227022.0A CN201610227022A CN105732320A CN 105732320 A CN105732320 A CN 105732320A CN 201610227022 A CN201610227022 A CN 201610227022A CN 105732320 A CN105732320 A CN 105732320A
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- tower
- chdm
- rectifying
- rectifying column
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- 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
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a purifying method for 1,4-cyclohexanedimethanol.The purifying method comprises the following steps that crude 1,4-cyclohexanedimethanol and sodium hydroxide are added in a rectifying column bottom; rectifying starts to be performed under the vacuum condition, the rectifying column bottom temperature is 220 DEG C-240 DEG C, and when the column top temperature reaches 190 DEG C-205 DEG C, fractions start to be collected; when the column top temperature exceeds 205 DEG C, rectifying is stopped.According to 1,4-cyclohexanedimethanol obtained through the purifying method, the saponification value of the product can be greatly decreased.
Description
Technical field
The present invention relates to a kind of rectificating method, the method particularly reducing saponification number during rectification.
Background technology
1,4-CHDM mainly for the production of various polyester and copolyester, as PETG, SPCT,
PCTG and PCTA.1,4-CHDM and the p phthalic acid esterification with dicarboxylic acids feature, warp
It is used for after polycondensation producing polyester fiber, there is the features such as relative density is little, fusing point is high, good electrical property；Use
The pet resin of 1,4-CHDM modification by copolymerization, the crystalline rate of its product is relatively
Slowly, the most also having good processing and physical property, the purposes of 1,4-CHDM maximum is to produce
PETG (glycol modified PET resin), PETG be used for producing thermoforming food container, bottle and
Tank, pharmaceutical product packaging material.
1,4-CHDM crude product obtained by technique, can obtain purity ＞ 99.9% by rectification at present, but
Now product saponification number is higher, more than 0.60mgKOH/g, limits the development of product downstream.Existing
In purifying process, in order to reduce the saponification number of product, often through increasing the tower height method with the raising number of plates,
But the method often reduces product yield, affects economic benefit.Therefore finding a kind of does not affect yield
Meanwhile, the method reducing 1,4-CHDM saponification number is extremely urgent.
Summary of the invention
The invention aims to provide the purification process of a kind of 1,4-CHDM, including following step
Rapid:
A () adds 1,4 cyclohexane dimethanol crude product and sodium hydroxide in tower bottom of rectifying tower；
B () starts rectification under vacuum, rectifying column column bottom temperature is 220～240 DEG C, works as tower top temperature
After reaching 190～205 DEG C, start to collect fraction；
C (), after tower top temperature is more than 205 DEG C, stops rectification；
In step (a), sodium hydroxide is sodium hydrate solid or sodium hydroxide water that mass concentration is 30～50%
Solution；At the end of rectification, the fraction of collection is 1,4-CHDM after purification.
Further, before adding sodium hydroxide before (a) step, 1,4-CHDM crude product is also included
The determination step of middle ester impurities content, in the input amount of sodium hydroxide and crude product ester impurities content mole
Ratio is 0.8～1.5:1.
Further, the tower height of described rectifying column is 12～22m, and tower diameter is 0.8m.
Further, in rectifying column, vacuum is-0.095～-1MPa.
Technical scheme has following notable beneficial effect: by the purification process of the present invention, not shadow
While ringing former handicraft product yield and product quality, substantially increase product quality so that product saponification number
Index ＜ 0.20mgKOH/g.
Detailed description of the invention
The present invention is further described below by enumerating the example solving technical problem:
In the present invention, the milli of potassium hydroxide needed for saponification number refers to saponification every gram 1,4-CHDM product
Grams.1,4-CHDM crude product employed in following embodiment is with a batch of crude product, this batch
After testing, purity 98.67%, saponification number 1.10mgKOH/g, moisture 0.06%, esters content is about for secondary crude product
It is 0.41%.
Example 1
In tower bottom of rectifying tower, put into 1t 1,4-CHDM crude product, use tower height 15m, tower diameter 0.8m
Rectifying column, intensification rectifying column, open vacuum pump, make the vacuum of tower reach-0.095～-1MPa, at the bottom of tower temperature
Degree is 230 DEG C, when tower top temperature reaches 200 DEG C, starts to collect 1,4-CHDM and enters finished pot,
When tower top temperature is more than 205 DEG C, stops rectification, obtain product 0.945t, yield 94.5%, after testing,
Product purity 99.8%, saponification number 0.38mgKOH/g, moisture 0.06%.
Example 2
In tower bottom of rectifying tower, put into 1t 1,4-CHDM crude product, use tower height 22m, tower diameter 0.8m
Rectifying column, intensification rectifying column, open vacuum pump, make the vacuum of tower reach-0.095～-1MPa, at the bottom of tower temperature
Degree is 230 DEG C, when tower top temperature reaches 200 DEG C, starts to collect 1,4-CHDM and enters finished pot,
When tower top temperature is more than 205 DEG C, stops rectification, obtain product 0.805t, yield 80.5%, after testing,
Product purity 99.9%, saponification number 0.19mgKOH/g, moisture 0.06%.
Example 3
In tower bottom of rectifying tower, put into 1t crude product 1,4-CHDM, add 0.96kgNaOH solid (alkali
With ester impurities mol ratio=1:1), use tower height 15m, the rectifying column of tower diameter 0.8m, intensification rectifying column, open
Opening vacuum pump, make the vacuum of tower reach-0.095～-1MPa, column bottom temperature is 240 DEG C, when tower top temperature reaches
To 195 DEG C, start to collect 1,4-CHDM and enter finished pot, when tower top temperature is more than 205 DEG C,
Stop rectification, obtain product 0.938t, yield 93.8%, after testing, and product purity 99.8%, saponification number 0.37
MgKOH/g, moisture 0.05%.
Example 4
In tower bottom of rectifying tower, put into 1t crude product 1,4-CHDM, add 3.20kg 30%NaOH (alkali
With ester impurities mol ratio=1:1), use tower height 15m, the rectifying column of tower diameter 0.8m, intensification rectifying column, open
Opening vacuum pump, make the vacuum of tower reach-0.095～-1MPa, column bottom temperature is 220 DEG C, when tower top temperature reaches
To 190 DEG C, start to collect 1,4-CHDM and enter finished pot, when tower top temperature is more than 205 DEG C,
Stop rectification, obtain product 0.948t, yield 94.8%, after testing, and product purity 99.9%, saponification number 0.09
MgKOH/g, moisture 0.11%.
Example 5
In tower bottom of rectifying tower, put into 1t crude product 1,4-CHDM, add 1.92kg50%NaOH (alkali
With ester impurities mol ratio=1:1), use tower height 15m, the rectifying column of tower diameter 0.8m, intensification rectifying column, open
Opening vacuum pump, make the vacuum of tower reach-0.095～-1MPa, column bottom temperature is 230 DEG C, when tower top temperature reaches
To 200 DEG C, start to collect 1,4-CHDM and enter finished pot, when tower top temperature is more than 205 DEG C,
Stop rectification, obtain product 0.943t, yield 94.3%, after testing, and product purity 99.8%, saponification number 0.10
MgKOH/g, moisture 0.08%.
Example 6
In tower bottom of rectifying tower, put into 1t crude product 1,4-CHDM, add 1.54kg50%NaOH (alkali
With ester impurities mol ratio=0.8:1), employing tower height 15m, the rectifying column of tower diameter 0.8m, intensification rectifying column,
Opening vacuum pump, make the vacuum of tower reach-0.095～-1MPa, column bottom temperature is 230 DEG C, works as tower top temperature
Reach 200 DEG C, start to collect 1,4-CHDM and enter finished pot, when tower top temperature is more than 205 DEG C,
Stop rectification, obtain product 0.941t, yield 94.1%, after testing, and product purity 99.7%, saponification number 0.30
MgKOH/g, moisture 0.08%.
Example 7
In tower bottom of rectifying tower, put into 1t crude product 1,4-CHDM, add 2.88kg50%NaOH (alkali
With ester impurities mol ratio=1.5:1) employing tower height 15m, the rectifying column of tower diameter 0.8m, intensification rectifying column,
Opening vacuum pump, make the vacuum of tower reach-0.095～-1MPa, column bottom temperature is 230 DEG C, works as tower top temperature
Reach 200 DEG C, start to collect 1,4-CHDM and enter finished pot, when tower top temperature is more than 205 DEG C,
Stop rectification, obtain product 0.941t, yield 94.1%, after testing, and product purity 99.80%, saponification number
0.09mgKOH/g, moisture 0.08%.
Example 8
In tower bottom of rectifying tower, put into 1t crude product 1,4-CHDM, add 2.88kg50%NaOH (alkali
With ester impurities mol ratio=1:1) use tower height 12m, the rectifying column of tower diameter 0.8m, intensification rectifying column, open
Opening vacuum pump, make the vacuum of tower reach-0.095～-1MPa, column bottom temperature is 230 DEG C, when tower top temperature reaches
To 200 DEG C, start to collect 1,4-CHDM and enter finished pot, when tower top temperature is more than 205 DEG C,
Stop rectification, obtain product 0.951t, yield 95.1%, after testing, and product purity 99.30%, saponification number
0.12mgKOH/g, moisture 0.10%.
Above-described embodiment only for technology design and the feature of the present invention are described, its object is to allow and is familiar with this skill
The personage of art will appreciate that present disclosure and implements according to this, can not limit the protection model of the present invention with this
Enclose.All equivalence changes made according to spirit of the invention or modification, all should contain the protection in the present invention
Within the scope of.
Claims (4)
1. a purification process for 1,4-CHDM, comprises the following steps:
A () adds 1,4 cyclohexane dimethanol crude product and sodium hydroxide in tower bottom of rectifying tower；
B () starts rectification under vacuum, rectifying column column bottom temperature is 220～240 DEG C, after tower top temperature reaches 190～205 DEG C, starts to collect fraction；
C (), after tower top temperature is more than 205 DEG C, stops rectification；
In step (a), sodium hydroxide is sodium hydrate solid or sodium hydrate aqueous solution that mass concentration is 30～50%；At the end of rectification, the fraction of collection is 1,4-CHDM after purification.
The most according to claim 1 a kind of 1, the purification process of 4-cyclohexanedimethanol, it is characterized in that: before adding sodium hydroxide before (a) step, also include 1, the determination step of ester impurities content in 4-cyclohexanedimethanol crude product, the input amount of sodium hydroxide is 0.8～1.5:1 with the mol ratio of ester impurities content in crude product.
The purification process of a kind of 1,4-CHDM the most according to claim 1, it is characterised in that: the tower height of described rectifying column is 12～22m, and tower diameter is 0.8m.
The purification process of a kind of 1,4-CHDM the most according to claim 1, it is characterised in that: in rectifying column, vacuum is-0.095～-1MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610227022.0A CN105732320A (en) | 2016-04-13 | 2016-04-13 | Purifying method for 1,4-cyclohexanedimethanol |
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| CN201610227022.0A CN105732320A (en) | 2016-04-13 | 2016-04-13 | Purifying method for 1,4-cyclohexanedimethanol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776271A (en) * | 2017-11-13 | 2019-05-21 | 中国石油天然气股份有限公司 | The method of purification and discoloration method of 1,4-CHDM crude product |
| CN116099221A (en) * | 2023-02-21 | 2023-05-12 | 江苏虹港石化有限公司 | 1, 4-cyclohexanedimethanol purification device and purification method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008247742A (en) * | 2007-03-07 | 2008-10-16 | Ube Ind Ltd | Purification method for 1,6-hexanediol |
| CN101765578A (en) * | 2007-07-30 | 2010-06-30 | 陶氏环球技术公司 | C 6-C 16The process for purification of aliphatic diol |
-
2016
- 2016-04-13 CN CN201610227022.0A patent/CN105732320A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008247742A (en) * | 2007-03-07 | 2008-10-16 | Ube Ind Ltd | Purification method for 1,6-hexanediol |
| CN101765578A (en) * | 2007-07-30 | 2010-06-30 | 陶氏环球技术公司 | C 6-C 16The process for purification of aliphatic diol |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776271A (en) * | 2017-11-13 | 2019-05-21 | 中国石油天然气股份有限公司 | The method of purification and discoloration method of 1,4-CHDM crude product |
| CN109776271B (en) * | 2017-11-13 | 2022-07-05 | 中国石油天然气股份有限公司 | Purification method and decolorization method of 1, 4-cyclohexanedimethanol crude product |
| CN116099221A (en) * | 2023-02-21 | 2023-05-12 | 江苏虹港石化有限公司 | 1, 4-cyclohexanedimethanol purification device and purification method |
| CN116099221B (en) * | 2023-02-21 | 2023-10-17 | 江苏虹港石化有限公司 | 1, 4-cyclohexanedimethanol purification device and purification method |
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Application publication date: 20160706 |