CN105251536A - Modified composite acidic ion resin for bisphenol F synthesis - Google Patents
Modified composite acidic ion resin for bisphenol F synthesis Download PDFInfo
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- CN105251536A CN105251536A CN201510750029.6A CN201510750029A CN105251536A CN 105251536 A CN105251536 A CN 105251536A CN 201510750029 A CN201510750029 A CN 201510750029A CN 105251536 A CN105251536 A CN 105251536A
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- bisphenol
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- acidic ion
- ion exchange
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Abstract
The invention discloses a modified composite acidic ion resin for bisphenol F synthesis. The preparation method comprises the following steps: treating and reacting a 732 strong-acid ion exchange resin, lithium chloride, phosphoric acid and aluminum trichloride, thereby obtaining a novel modified composite acidic ion resin. The modified composite acidic ion resin disclosed by the invention has the advantages that the activity of the modified composite catalyst is high; the modified composite catalyst is simple in preparation process and long in service life; and the used raw materials are simple and readily available, simple in reaction steps and easy to synthesize. Therefore, the designed synthesis of the modified composite catalyst has good industrial application prospects.
Description
Technical field
The present invention relates to a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis and preparation method thereof; Bisphenol F (BPF) is a kind of important Organic Chemicals.In the actual production of Bisphenol F, catalyst plays the role of particular importance, and therefore the design of efficient catalyst is the key of Bisphenol F synthesis.Belong to chemical material and drug world.
Background technology
Bisphenol F is the bisphenol type compounds by phenol and formaldehyde condensation, is a kind of novel organic work raw material of exploitation eighties of last century eighties, is mainly used in the modifier of low viscosity epoxy resin, specialty polyesters resin raw material and phenolic resins and stabilizing agent etc.Participated in the phenol-formaldehyde resin modified manufactured by Bisphenol F, greatly can improve the processing characteristics of phenolic resins, mechanical property and electrical property, therefore obtain and apply comparatively widely.And catalyst is wherein one of important process condition in Bisphenol F synthesis technique.At present preferably method is catalyst with phosphoric acid, but there is the problems such as high phenol formaldehyde ratio, low yield, product postprocessing are complicated.
Ion exchange resin is a kind of polyelectrolyte of water insoluble, bronsted lowry acids and bases bronsted lowry, has the performance of acid, alkali.Because ion exchange resin has high activity, reaction condition is gentle, there is not corrosiveness to equipment, and after regeneration, the advantage such as reusable, obtains both at home and abroad investigation and application widely.
In order to solve the difficulty in Bisphenol F synthesis, the advantage of coupled ion exchanger resin simultaneously, the present invention is based on 732 strong-acid ion exchange resins, and a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis of design and synthesis, this modified composite catalyst is not yet reported at present.
Summary of the invention
The invention discloses a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis.Find in our study, the catalytic performance that this modification combination of acidic ion exchange resin synthesizes for Bisphenol F is better.
The invention provides a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis, it is characterized in that, comprise the steps: 732 strong-acid ion exchange resins to soak 2 hours at 1.5mol/L lithium chloride solution, add hot reflux 1-4 hour afterwards; Then, then soak 2 hours with 3.5mol/L phosphoric acid solution, add alchlor, 80-120 DEG C adds thermal agitation hour afterwards, is cooled to room temperature.Suction filtration, then washs 3 times with distilled water, the solid matter obtained, and under 95 DEG C of conditions, vacuum drying 7 hours, obtains solid catalyst.
Detailed description of the invention
As described above is often applied in the synthesis technique of Bisphenol F.The combination of acidic ion exchange resin of this modification provided by the invention can significantly improve catalyst activity, and the preparation technology of catalyst is simple, catalyst long service life.
Below, applicant to invention has been specific experiment, and describe in detail modified acidic ion resin be applied in Bisphenol F synthesis in the middle of experimentation.These only for elaborating the present invention, and limit scope of invention never in any form.
Embodiment one: a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis, comprises following processing step:
732 strong-acid ion exchange resins are soaked 2 hours at 1.5mol/L lithium chloride solution, adds hot reflux afterwards 1 hour; Then, then soak 2 hours with 3.5mol/L phosphoric acid solution, add alchlor, 80 DEG C add thermal agitation 1 hour afterwards, are cooled to room temperature.Suction filtration, then washs 3 times with distilled water, the solid matter obtained, and under 95 DEG C of conditions, vacuum drying 7 hours, obtains solid catalyst.
By gained catalyst application in Bisphenol F synthesis: phenol (0.4mol), acid ion resin (4g) are joined in reaction vessel, stirred at ambient temperature is even, add 200mL toluene, more slowly add 37% formalin, be heated to 110 DEG C.Reaction time is 6 hours.The reactant liquor layering will obtained after reaction terminates, oil reservoir is the thick product of reaction.Thick for gained product is revolved and steams recycling design, decompression distillation and reclaim remaining phenol, the toluene of surplus products recovery again crystallization once, just can obtain 4,4 dihydroxydiphenyl methane.Productive rate: 72%.
Embodiment two: a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis, comprises following processing step:
732 strong-acid ion exchange resins are soaked 2 hours at 1.5mol/L lithium chloride solution, adds hot reflux afterwards 4 hours; Then, then soak 2 hours with 3.5mol/L phosphoric acid solution, add alchlor, 120 DEG C add thermal agitation 1 hour afterwards, are cooled to room temperature.Suction filtration, then washs 3 times with distilled water, the solid matter obtained, and under 95 DEG C of conditions, vacuum drying 7 hours, obtains solid catalyst.
By gained catalyst application in Bisphenol F synthesis: phenol (0.4mol), acid ion resin (4g) are joined in reaction vessel, stirred at ambient temperature is even, add 200mL toluene, more slowly add 37% formalin, be heated to 110 DEG C.Reaction time is 6 hours.The reactant liquor layering will obtained after reaction terminates, oil reservoir is the thick product of reaction.Thick for gained product is revolved and steams recycling design, decompression distillation and reclaim remaining phenol, the toluene of surplus products recovery again crystallization once, just can obtain 4,4 dihydroxydiphenyl methane.Productive rate: 78%.
Embodiment three: a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis, comprises following processing step:
By 732 strong-acid ion exchange resins, soak 2 hours at 1.5mol/L lithium chloride solution, add hot reflux afterwards 2 hours; Then, then soak 2 hours with 3.5mol/L phosphoric acid solution, add alchlor, 100 DEG C add thermal agitation 1 hour afterwards, are cooled to room temperature.Suction filtration, then washs 3 times with distilled water, the solid matter obtained, and under 95 DEG C of conditions, vacuum drying 7 hours, obtains solid catalyst.
By gained catalyst application in Bisphenol F synthesis: phenol (0.4mol), acid ion resin (4g) are joined in reaction vessel, stirred at ambient temperature is even, add 200mL toluene, more slowly add 37% formalin, be heated to 110 DEG C.Reaction time is 6 hours.The reactant liquor layering will obtained after reaction terminates, oil reservoir is the thick product of reaction.Thick for gained product is revolved and steams recycling design, decompression distillation and reclaim remaining phenol, the toluene of surplus products recovery again crystallization once, just can obtain 4,4 dihydroxydiphenyl methane.Productive rate: 75%.
Claims (2)
1. the invention provides a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis.
2. a kind of modification combination of acidic ion exchange resin for Bisphenol F synthesis described in; It is characterized in that, comprise the steps: 732 strong-acid ion exchange resins to soak 2 hours at 1.5mol/L lithium chloride solution, add hot reflux 1-4 hour afterwards; Then, then soak 2 hours with 3.5mol/L phosphoric acid solution, add alchlor, 80-120 DEG C adds thermal agitation 1 hour afterwards, is cooled to room temperature.Suction filtration, then washs 3 times with distilled water, the solid matter obtained, and under 95 DEG C of conditions, vacuum drying 7 hours, obtains solid catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510750029.6A CN105251536A (en) | 2015-11-06 | 2015-11-06 | Modified composite acidic ion resin for bisphenol F synthesis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510750029.6A CN105251536A (en) | 2015-11-06 | 2015-11-06 | Modified composite acidic ion resin for bisphenol F synthesis |
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| CN105251536A true CN105251536A (en) | 2016-01-20 |
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| CN201510750029.6A Pending CN105251536A (en) | 2015-11-06 | 2015-11-06 | Modified composite acidic ion resin for bisphenol F synthesis |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491879A (en) * | 2011-11-14 | 2012-06-13 | 湘潭大学 | Preparation method for bisphenol F |
| CN103896742A (en) * | 2014-01-21 | 2014-07-02 | 湘潭大学 | Method for catalytic synthesis of bisphenol F by using cation exchange resin immobilized ionic liquid |
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2015
- 2015-11-06 CN CN201510750029.6A patent/CN105251536A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491879A (en) * | 2011-11-14 | 2012-06-13 | 湘潭大学 | Preparation method for bisphenol F |
| CN103896742A (en) * | 2014-01-21 | 2014-07-02 | 湘潭大学 | Method for catalytic synthesis of bisphenol F by using cation exchange resin immobilized ionic liquid |
Non-Patent Citations (3)
| Title |
|---|
| 张文雯等: "双酚F合成反应的负载型树脂催化剂研究", 《化学世界》 * |
| 张文雯等: "改性阳离子交换树脂催化合成双酚F", 《化工进展》 * |
| 陈桂等: "改性阳离子交换树脂的制备、表征及催化合成双酚F", 《离子交换与吸附》 * |
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Application publication date: 20160120 |