CN102795966B - Method for controlling polymerization in rectification process of 1,4-cyclohexanedimethanol - Google Patents
Method for controlling polymerization in rectification process of 1,4-cyclohexanedimethanol Download PDFInfo
- Publication number
- CN102795966B CN102795966B CN201110134925.1A CN201110134925A CN102795966B CN 102795966 B CN102795966 B CN 102795966B CN 201110134925 A CN201110134925 A CN 201110134925A CN 102795966 B CN102795966 B CN 102795966B
- Authority
- CN
- China
- Prior art keywords
- tower
- rectifying
- cyclohexanedimethanol
- rectification
- cyclohexane dimethanol
- 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.)
- Active
Links
Abstract
The invention relates to a method for controlling polymerization in a rectification process of 1,4-cyclohexanedimethanol. A rectification method is mainly adopted. The method is characterized in that a rectification tower with the height of 12 meters and the diameter of 0.8 meter is used, and 2,5-ditertbutyl hydroquinone polymerization inhibitor is rectified in vacuum of 0.100MPa below zero. The invention has the advantages that the colorless and transparent 1,4-cyclohexanedimethanol of which the content is more than 99.9 percent can be obtained by adopting the method. The method is adopted by the following reasons that when a crude product is rectified, because the boiling point of the 1,4-cyclohexanedimethanol is 286 DEG C, the 1,4-cyclohexanedimethanol is dehydrated and polymerized very seriously at a high temperature, and the yield (the rectification yield is about 90 percent) of the 1,4-cyclohexanedimethanol is greatly affected; and by using the rectification tower with the height of 12 meters and the diameter of 0.8 meter and adding the 2,5-ditertbutyl hydroquinone polymerization inhibitor in the vacuum of 0.100MPa below zero, high-temperature dehydration and polymerization of the 1,4-cyclohexanedimethanol are greatly reduced, and the rectification yield is over 97 percent.
Description
Technical field
The present invention relates to a kind of method of 1,4 cyclohexane dimethanol rectifying, specifically a kind of method that adopts rectifying tower to realize the 1,4 cyclohexane dimethanol rectifying of rectifying.
Background technology
Saturation type vibrin taking 1,4 cyclohexane dimethanol as raw material production is used in coating and coating has a lot of good characteristics, can make the crystallinity of vibrin improve, and is that stability, the sintering resistance of powder coating improves.1,4 cyclohexane dimethanol can also be used for the production of the unsaturated polyester resin that sheet material and film use with compound in addition, and product has satisfactory stability, electrical property and erosion resistance.Be widely used in and produce film, use for electronic products resin and insulated wire etc.
The Isosorbide-5-Nitrae cyclohexanedimethanol crude product that reaction directly obtains, does not reach content > 99.9%, and color and luster is water white requirement, has limited to a certain extent the development of Isosorbide-5-Nitrae cyclohexanedimethanol and derived product thereof.In order to meet the demand in market, also in order to improve the Liao Wo company competitiveness of product in market, need be to the frequent rectification process of crude product.
286 DEG C of 1,4 cyclohexane dimethanol boiling points, the polymerization of can dewatering under high temperature is more serious, rectification yield is only 90% left and right, so no matter consider from development of company or economic benefit, in research control 1,4 cyclohexane dimethanol rectifying, the control of polymerization is imperative.
Summary of the invention
Main task of the present invention is to provide a kind of control polymerization in 1,4 cyclohexane dimethanol rectifying method, and specifically high, the color and luster of content is the method for controlling polymerization in water white 1,4 cyclohexane dimethanol rectifying.
In order to solve above technical problem, a kind of control 1 of the present invention, the method of polymerization in 4-cyclohexanedimethanol rectifying, the main method that adopts rectifying, it is characterized in that: described in select tower height 12m, the rectifying tower of tower diameter 0.8m, under the vacuum condition of-0.100MPa, select the rectifying of 2,5 di tert butyl hydroquinone stopper.
Further, described 2,5 di tert butyl hydroquinone stopper add-on is 0.05% of crude product quality.
The invention has the advantages that: adopt above-mentioned technique, can obtain content > 99.9%, color and luster is water white 1,4 cyclohexane dimethanol.Adopt the reason of this technique to be: to crude product through rectifying, 286 DEG C of 1,4 cyclohexane dimethanol boiling points, the polymerization of can dewatering under high temperature is very serious, has greatly affected the yield (rectification yield 90% left and right) of product, by the present invention, selecting tower height 12m, the rectifying tower of tower diameter 0.8m, under the vacuum condition of-0.100MPa, by stopper 2,5-di-tert-butyl hydroquinone's interpolation, greatly reduce the generation of Isosorbide-5-Nitrae-hexanaphthene high temperature dehydration polymerization, rectification yield reaches more than 97%.
Embodiment
Technical problem to be solved by this invention is achieved through the following technical solutions:
The crude product of reaction gained is transported to rectifying tower storage tank, add 2 of respective amount, 5-di-tert-butyl hydroquinone (crude product quality 0.05%), rectifying tower is opened thermal oil and is heated up, and opens vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, the hot water condensation of 60 DEG C of left and right for tower top cut out, the 1,4 cyclohexane dimethanol maintaining like this after separation enters finished product storage tank under liquid state.In the time that column bottom temperature approaches 210 DEG C, fluid not substantially, stops rectifying.
Example 1:
In rectifying tower storage tank, add the 1,4 cyclohexane dimethanol into 2t, adopt tower height 12m, the rectifying tower of tower diameter 0.8m carries out rectifying, unlatching thermal oil heats up, and opens vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, and tower top does not stop rectifying when fluid, obtains 1.81t clear, colorless 1,4-cyclohexanedimethanol, chromatogram content 99.9%.
Example 2:
In rectifying tower storage tank, add the 1,4 cyclohexane dimethanol into 2t, adopt tower height 22m, the rectifying tower of tower diameter 0.8m carries out rectifying, unlatching thermal oil heats up, and opens vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, and tower top does not stop rectifying when fluid, obtains 1.23t clear, colorless 1,4-cyclohexanedimethanol, chromatogram content 99.9%.
Example 3:
In rectifying tower storage tank, add the 1,4 cyclohexane dimethanol into 2t, add 1kg Resorcinol, adopt tower height 12m, the rectifying tower of tower diameter 0.8m carries out rectifying, opens thermal oil and heats up, unlatching vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, tower top does not stop rectifying when fluid, obtain 1.88t clear, colorless 1,4 cyclohexane dimethanol, chromatogram content 99.9%.
Example 4:
In rectifying tower storage tank, add the 1,4 cyclohexane dimethanol into 2t, add 1kg para benzoquinone, adopt tower height 12m, the rectifying tower of tower diameter 0.8m carries out rectifying, opens thermal oil and heats up, unlatching vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, tower top does not stop rectifying when fluid, obtain 1.91t clear, colorless 1,4 cyclohexane dimethanol, chromatogram content 99.9%.
Example 5:
In rectifying tower storage tank, add the 1,4 cyclohexane dimethanol into 2t, add 1kg Trimethylhydroquinone, adopt tower height 12m, the rectifying tower of tower diameter 0.8m carries out rectifying, opens thermal oil and heats up, unlatching vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, tower top does not stop rectifying when fluid, obtain 1.93t clear, colorless 1,4 cyclohexane dimethanol, chromatogram content 99.9%.
Example 6:
In rectifying tower storage tank, add the 1,4 cyclohexane dimethanol into 2t, add 1kg MEHQ, adopt tower height 12m, the rectifying tower of tower diameter 0.8m carries out rectifying, opens thermal oil and heats up, unlatching vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, tower top does not stop rectifying when fluid, obtain 1.91t clear, colorless 1,4 cyclohexane dimethanol, chromatogram content 99.9%.
Example 7:
In rectifying tower storage tank, add the 1,4 cyclohexane dimethanol into 2t, add 1kg2,5-di-tert-butyl hydroquinone, adopts tower height 12m, and the rectifying tower of tower diameter 0.8m carries out rectifying, unlatching thermal oil heats up, and opens vacuum basis, the vacuum tightness of tower is reached-0.100MPa, maintain 180 DEG C-190 DEG C of tower top temperatures, column bottom temperature is at 200-210 DEG C, and tower top does not stop rectifying when fluid, obtains 1.95t clear, colorless 1,4-cyclohexanedimethanol, chromatogram content 99.9%.
Claims (1)
1. control a method for polymerization in 1,4 cyclohexane dimethanol rectifying, mainly adopt the method for rectifying, it is characterized in that: described in select tower height 12m, the rectifying tower of tower diameter 0.8m, under the vacuum condition of-0.100MPa, select the rectifying of 2,5 di tert butyl hydroquinone stopper; Described 2,5 di tert butyl hydroquinone stopper add-on is 0.05% of 1,4 cyclohexane dimethanol crude product quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110134925.1A CN102795966B (en) | 2011-05-24 | 2011-05-24 | Method for controlling polymerization in rectification process of 1,4-cyclohexanedimethanol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110134925.1A CN102795966B (en) | 2011-05-24 | 2011-05-24 | Method for controlling polymerization in rectification process of 1,4-cyclohexanedimethanol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102795966A CN102795966A (en) | 2012-11-28 |
| CN102795966B true CN102795966B (en) | 2014-09-03 |
Family
ID=47195308
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110134925.1A Active CN102795966B (en) | 2011-05-24 | 2011-05-24 | Method for controlling polymerization in rectification process of 1,4-cyclohexanedimethanol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102795966B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3207022B1 (en) | 2014-10-14 | 2020-01-29 | Ecolab USA Inc. | Reducing polymer fouling and agglomeration in acrylate/methacrylate processes |
| RU2715559C2 (en) | 2015-03-18 | 2020-03-02 | ЭКОЛАБ ЮЭсЭй ИНК. | Use of stable lipophilic hydroxylamine compounds to inhibit polymerisation of vinyl monomers |
| US9957209B2 (en) | 2015-03-31 | 2018-05-01 | Ecolab Usa Inc. | Use of quinone methides as antipolymerants for vinylic monomers |
| CN107532083A (en) | 2015-04-20 | 2018-01-02 | 艺康美国股份有限公司 | Steric hindrance quinhydrones is used for unsaturated monomer as anti-fouling agent |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033171A (en) * | 2007-04-16 | 2007-09-12 | 清华大学 | Technique of extracting 1,3-dihydroxypropane prepared by fermentation method |
| CN101274875A (en) * | 2007-03-30 | 2008-10-01 | 中国石油天然气股份有限公司 | Composite type polymerization inhibitor for butadiene purification and refinement |
| CN101591216A (en) * | 2009-07-10 | 2009-12-02 | 北京斯伯乐科学技术研究院 | A kind of high-efficiency multi-functional polymerization inhibitor and using method thereof that is used for butadiene extraction unit |
-
2011
- 2011-05-24 CN CN201110134925.1A patent/CN102795966B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274875A (en) * | 2007-03-30 | 2008-10-01 | 中国石油天然气股份有限公司 | Composite type polymerization inhibitor for butadiene purification and refinement |
| CN101033171A (en) * | 2007-04-16 | 2007-09-12 | 清华大学 | Technique of extracting 1,3-dihydroxypropane prepared by fermentation method |
| CN101591216A (en) * | 2009-07-10 | 2009-12-02 | 北京斯伯乐科学技术研究院 | A kind of high-efficiency multi-functional polymerization inhibitor and using method thereof that is used for butadiene extraction unit |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102795966A (en) | 2012-11-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102795966B (en) | Method for controlling polymerization in rectification process of 1,4-cyclohexanedimethanol | |
| CN109574816A (en) | A kind of dichloro pinacoline production technology | |
| CN104058923B (en) | The method of one-sided line extraction azeotropic distillation separating alcohol-water-isopropyl benzene mixing solutions | |
| CN103951793A (en) | Method for producing unsaturated polyester resin by using glycerinum | |
| CN103055530A (en) | Solvent reinforced transformation thermal coupling rectification system for separating cyclohexanone and phenol | |
| CN102320943B (en) | Preparation method of benzaldehyde | |
| CN102701908B (en) | A kind of calcium legal system is for the technique of neopentyl glycol | |
| CN107011151B (en) | Method for improving benzaldehyde selectivity in toluene liquid-phase catalytic oxidation process | |
| CN105585683A (en) | Method for preparing melamine formaldehyde resin flocculating agent | |
| CN103087094A (en) | Method and device for rectifying and purifying triethyl phosphate in batches | |
| CN104017189B (en) | A kind of preparation method without antimony polyester for bottle | |
| CN104829426A (en) | Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent | |
| CN104497275A (en) | Modified aromatic amine epoxy curing agent and preparation method thereof | |
| CN103304988B (en) | A kind of Impact-resistant high-temperature-resplastic plastic containing polyarylsulphone | |
| CN103601639A (en) | O-chlorobenzoic acid synthesis process | |
| CN106008241A (en) | Synthesis method for N,N-dimethylaminoethyl acrylate | |
| CN101838192A (en) | Trimethylacetic acid crude product refining process and device | |
| CN103467285B (en) | Method for reducing acidity of acetate | |
| CN106187765B (en) | Acetone, water separation equipment in a kind of two tower of rectifying removing vinyl acetate | |
| CN102585645A (en) | Anti-counterfeiting electrolytic aluminum coating and preparation method thereof | |
| CN102002303A (en) | Pure epoxy quickly-cured powder coating and production method thereof | |
| CN104610055A (en) | Preparation method for synthesizing propyl acetate by catalytic rectifying process | |
| CN101864256A (en) | Method for preparing composite adhesive | |
| CN104592170A (en) | Method for producing epoxy fatty acid methyl ester by taking illegal cooking oil as raw material | |
| CN103265430A (en) | Preparation method of hydroxypropyl acrylate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 226500, Jiangsu Province, Nantong City, Rugao Shi Zhuang Town, new harbor village 24 groups (the former south side of the mulberry bridge) Patentee after: Jiangsu Heng Xiang Chemical Limited by Share Ltd Address before: 226500, Jiangsu Province, Nantong City, Rugao Shi Zhuang Town, new harbor village 24 groups (the former south side of the mulberry bridge) Patentee before: Jiangsu Heng-Xi'ang Chemical Co., Ltd. |