CN110981211B - Preparation method of polymer modified glass filler for rectification - Google Patents
Preparation method of polymer modified glass filler for rectification Download PDFInfo
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- CN110981211B CN110981211B CN201911417029.9A CN201911417029A CN110981211B CN 110981211 B CN110981211 B CN 110981211B CN 201911417029 A CN201911417029 A CN 201911417029A CN 110981211 B CN110981211 B CN 110981211B
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- glass filler
- ketone
- rectification
- monomer
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/30—Loose or shaped packing elements, e.g. Raschig rings or Berl saddles, for pouring into the apparatus for mass or heat transfer
Abstract
The invention belongs to the technical field of modification of a filler for rectification, and particularly relates to a preparation method of a polymer modified glass filler for rectification. The modified glass filler has high thermal stability and chemical corrosion resistance, and has better stability when being used for rectification.
Description
Technical Field
The invention belongs to the technical field of modification of a rectifying filler, and particularly relates to a preparation method of a polymer modified glass filler for rectification.
Background
Common fillers in organic solvent rectification are glass and metal materials. The main component of the glass is silicon dioxide, the surface of the glass is rich in silicon hydroxyl, the polarity is large, and the defect of insufficient intermolecular force with most of conventional nonpolar organic solvents exists in rectification. Similarly, the surface of the metal material is often a metal oxide film, and similar disadvantages exist in rectification. Therefore, in the rectification process involving organic solvents, a very high packed column is often required to achieve the desired separation.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a polymer modified glass filler for rectification, which comprises the following steps: by utilizing the bonding reaction between silicon hydroxyl on the surface of the glass filler and organic molecules, molecular chains with a polyether-ether-ketone structure are grafted on the surface of the glass filler in a reaction way,
concretely, mixing glass filler, alkali, monomer with ketone group and diphenol monomer in a dispersant, heating for reaction, filtering out the glass filler, cleaning and drying to obtain the glass filler grafted with a polyether-ether-ketone molecular chain structure, namely the polymer modified glass filler for rectification,
wherein the glass filler is hollow cylindrical ground glass filler,
the base is sodium hydrogen (sodium hydride),
the monomer with ketone group is ketone substituted by halogenated phenyl, and the ketone molecule has two halogenated phenyl, such as 4,4' -difluorobenzophenone,
the diphenol monomer is aliphatic chain-containing diphenol monomer or aromatic diphenol monomer,
the reaction temperature during the temperature rise reaction is 45-65 ℃,
preferably, the method comprises the following steps: firstly adding the glass filler and part of alkali into the dispersant, adding the monomer with ketone groups under the heating and stirring state, cooling after stirring and reacting for a period of time, adding the diphenol monomer and the rest alkali, heating and stirring for reacting fully, filtering out the glass filler, washing with clear water and drying.
The technical scheme is that the surface of glass is grafted and modified by adopting special polyether-ether-ketone plastic to serve as a rectifying column filler, and the preparation method is characterized in that hydroxyl on the surface of the glass is bonded with a polyether-ether-ketone structure, so that a polyether-ether-ketone coating is formed on the surface of the glass filler, the glass filler has high thermal stability and chemical corrosion resistance, the glass filler can work at the traditional rectifying temperature (within 200 ℃) and in a conventional solvent with higher concentration, and tests show that the filler with the same size and the surface-modified glass filler only need the filler height of 1/5-1/3, so that the effect of the traditional glass or metal filler can be achieved.
Drawings
FIG. 1 is an infrared spectrum of a polyetheretherketone-modified glass filler finally prepared in example,
therein, 1652cm -1 Representing the C-O double bond vibrational band of polyetheretherketone, 1226cm -1 Representing asymmetric stretching vibration band of ether bond, which indicates the surface of glass fillerThe polyether-ether-ketone molecular chain is grafted on the graft,
atlas 2800cm -1 To 3200cm -1 The absence of bands in the interval indicates that the product is essentially free of hydroxyl groups, i.e. hydroxyl groups on the surface of the glass filler have been bonded.
Detailed Description
Taking 300g of dry hollow cylindrical ground glass filler (the outer diameter is 5mm, the inner diameter is 3.5mm, and the height (axial length) is 6mm), adding the dry hollow cylindrical ground glass filler into 700mL of anhydrous methyl pyrrolidone, magnetically stirring the mixture (30 r/min), adding 0.5g of NaH (added in the form of mineral oil with the NaH mass fraction of 60%), heating the mixture to 50 ℃ and stirring the mixture for 30 minutes, adding 10g of 4,4' -difluorobenzophenone (the 4,4' -difluorobenzophenone is excessive compared with the hydroxyl on the glass surface, so that the hydroxyl on the glass surface is basically completely reacted, and the remaining 4,4' -difluorobenzophenone participates in the subsequent reaction for generating a polyether ether ketone polymer chain), keeping the temperature and stirring the mixture for 30 minutes, reducing the temperature to 20 ℃, adding 4g of hydroquinone and stirring the mixture for 10 minutes, then adding 0.3g of NaH (added in the form of mineral oil with the NaH mass fraction of 60%), after the addition, the temperature was raised to 50 ℃ and the mixture was stirred for 1 hour, after the reaction was completed, the mixture was cooled to 20 ℃ and 3mL of distilled water was added dropwise to quench the excess NaH. Filtering out the glass filler, rinsing with distilled water for 3 times, placing the obtained filler into a blast oven at 60 ℃ for drying for 4 hours to obtain the polyether-ether-ketone modified glass filler, and detecting by infrared spectroscopy as shown in figure 1.
The reaction formula is as follows:
in the reaction, sodium hydride (sodium hydrogen) is used as alkali, sodium hydrogen reacts with silanol to generate sodium silanol and hydrogen, and a small amount of hydrogen can be directly separated from a reaction system, so that water is prevented from being introduced in the reaction; meanwhile, sodium hydrogen is also used when the disodium p-phenoxide is prepared, the phenolic hydroxyl of the p-diphenol reacts with the sodium hydrogen to obtain sodium p-diphenol, and then the sodium p-diphenol reacts with the monofluorobenzophenone bonded to the surface of the glass, so that the generation of a byproduct of water is avoided when the disodium p-phenoxide is prepared.
Destructive test
5g of the polyether-ether-ketone-modified glass filler prepared in the embodiment is added into 5mL of uniform mixtures of toluene/dichloromethane/ethyl acetate/n-hexane/n-butyl ketone/chloroform, the mixture is heated to 200 ℃ in a sealed tank (sealed mode) and is magnetically stirred (30 revolutions per minute) for 8 hours at the temperature, the mixture is cooled to 20 ℃ and then filtered, the obtained filtrate is subjected to GCMS test, impurities associated with 4,4' -difluorobenzophenone or hydroquinone are not detected, and the polyether-ether-ketone coating on the surface of the glass filler is stable and is not easy to decompose.
Claims (3)
1. A preparation method of polymer modified glass filler for rectification is characterized by comprising the following steps: the preparation method comprises the steps of utilizing bonding reaction between silicon hydroxyl on the surface of the glass filler and organic molecules to graft a molecular chain with a polyether-ether-ketone structure on the surface of the glass filler;
the preparation method specifically comprises the steps of mixing glass filler, alkali, a monomer with a ketone group and a diphenol monomer in a dispersing agent, heating to react at 45-65 ℃, filtering the glass filler, washing and drying to obtain the glass filler grafted with a polyether-ether-ketone molecular chain structure, namely the polymer modified glass filler for rectification; the monomer with the ketone group is ketone substituted by halogenated phenyl, and the molecule of the ketone has two halogenated phenyl; the diphenol monomer is an aliphatic chain-containing diphenol monomer and/or an aromatic diphenol monomer;
the preparation method further comprises the steps of adding the glass filler and part of alkali into the dispersing agent, adding the monomer with the ketone group under the heating and stirring state, cooling after stirring and reacting for a period of time, adding the diphenol monomer and the rest alkali, heating and stirring for reacting fully, filtering the glass filler, washing with clear water and drying.
2. The method of claim 1 for preparing a polymer modified glass filler useful for distillation, wherein: the glass filler is hollow cylindrical ground glass filler.
3. The method of claim 1 for preparing a polymer modified glass filler useful for rectification, wherein: the alkali is sodium hydride.
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| CN201911417029.9A CN110981211B (en) | 2019-12-31 | 2019-12-31 | Preparation method of polymer modified glass filler for rectification |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911417029.9A CN110981211B (en) | 2019-12-31 | 2019-12-31 | Preparation method of polymer modified glass filler for rectification |
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| CN110981211A CN110981211A (en) | 2020-04-10 |
| CN110981211B true CN110981211B (en) | 2022-08-12 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2822393A1 (en) * | 1978-05-23 | 1979-11-29 | Klaus J Prof Dr Ing Huettinger | Modifying the wetting properties of solid surfaces - by treatment with a modifier which grafts to the surface by covalent bonds |
| CN101356003A (en) * | 2005-12-16 | 2009-01-28 | 阿克佐诺贝尔公司 | Silica based material |
| CN102702798A (en) * | 2012-06-18 | 2012-10-03 | 中国船舶重工集团公司第七二五研究所 | Modified silica filler and preparation method thereof |
| CN105733180A (en) * | 2014-12-10 | 2016-07-06 | 黑龙江鑫达企业集团有限公司 | Preparation method of special coupling agent-treated SiO2-enhanced PEEK |
| CN108079982A (en) * | 2017-12-22 | 2018-05-29 | 苏州纳微科技有限公司 | A kind of modified silica-gel filler, preparation method and purposes |
-
2019
- 2019-12-31 CN CN201911417029.9A patent/CN110981211B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2822393A1 (en) * | 1978-05-23 | 1979-11-29 | Klaus J Prof Dr Ing Huettinger | Modifying the wetting properties of solid surfaces - by treatment with a modifier which grafts to the surface by covalent bonds |
| CN101356003A (en) * | 2005-12-16 | 2009-01-28 | 阿克佐诺贝尔公司 | Silica based material |
| CN102702798A (en) * | 2012-06-18 | 2012-10-03 | 中国船舶重工集团公司第七二五研究所 | Modified silica filler and preparation method thereof |
| CN105733180A (en) * | 2014-12-10 | 2016-07-06 | 黑龙江鑫达企业集团有限公司 | Preparation method of special coupling agent-treated SiO2-enhanced PEEK |
| CN108079982A (en) * | 2017-12-22 | 2018-05-29 | 苏州纳微科技有限公司 | A kind of modified silica-gel filler, preparation method and purposes |
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