CN1231302A - One stage synthesizing polyether sulfone resin by using dimethyl sulfone as solvent - Google Patents
One stage synthesizing polyether sulfone resin by using dimethyl sulfone as solvent Download PDFInfo
- Publication number
- CN1231302A CN1231302A CN 99103164 CN99103164A CN1231302A CN 1231302 A CN1231302 A CN 1231302A CN 99103164 CN99103164 CN 99103164 CN 99103164 A CN99103164 A CN 99103164A CN 1231302 A CN1231302 A CN 1231302A
- Authority
- CN
- China
- Prior art keywords
- solvent
- dimethyl sulfone
- resin
- polyether sulphone
- sulfone
- 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.)
- Pending
Links
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The one-step synthesis technology of polyether sulphone resin by using dimethyl sulfone as solvent is characterized by substituting sulfolane solvent with dimethyl sulfone, so that it not only can reduce the cost of synthetic polyether sulphone resin, but also can synthesize various polyether sulphone resins suitable for different requirements by means of regulating monomer mixing ratio.
Description
The present invention is that a kind of dimethyl sulfone of utilizing is solvent single stage method synthesizing polyether sulphone resin technology.
To synthesizing of polyethersulfone resin, two patents that we were applied in the past all are to adopt tetramethylene sulfone to make solvent, there are two problems that urgency is to be solved in past in producing always, the one, the tetramethylene sulfone price rises steadily, from original 7000 yuan/ton, increase to 40,000 ten thousand/ton, by 0.3 ton of resin consumption per ton then only this item raw materials cost just increase by 10,000 yuan.The 2nd, because the tetramethylene sulfone fusing point has only twenties degree, boiling point is high again, reclaims when making with extra care and can only distill with vacuum decompression, and not only complex process but also energy consumption are big.Also unfavorable to reducing cost.For addressing the above problem under the situation of also not having other industrial raw material at home, at first we have invented the technology of preparation dimethyl sulfone in another patent, achieve success the back we to use dimethyl sulfone instead be solvent, pass through the screening of polymerization technique again, by the adjusting of monomer blends ratio, can synthesize the various polyethersulfone resins that are suitable for different service requirementss.As being fit to the hydroxyl-terminated polyether sulfone that coating is used by excessive synthesizing of monomer bis-phenol-S; By excessive synthesizing of two chlorine being fit to the polyethersulfone that engineering plastics are used.Also can regulate molecular weight of product simultaneously by the control of the excessive degree of monomer (between 1: 1～1.3).Molecular weight maximum when mole ratio (1: 1) increases molecular weight with excessive number and constantly diminishes, thereby finished the present invention.Because dimethyl sulfone has only 1.5 ten thousand yuan/ton,, reach the purpose that reduces the resin cost so only raw materials cost of solvent can reduce more than 5000 yuan/ton.
Embodiment one
Logical nitrogen tube of thermometer and condensation water trap are being housed, in three mouthfuls of reaction flasks of agitator, add the 270.0g dimethyl sulfone earlier, add the promptly two chlorine excessive 1.0% of the two chlorine of 72.47g (0.2525mol) and 62.50g (0.25mol) bis-phenol-S then in turn, add again 60ml dimethylbenzene post-heating it is all dissolved and add when treating that temperature rises to 80 ℃ the alkaline solution (strength of solution is being advisable between 30～35%) that contains 20.0gNaOH continue heat temperature raising to 100 ℃ again more than system begin azeotropic, there are dimethylbenzene and water to be condensed simultaneously in the water trap, the upper strata refluxing xylene, lower layer of water is constantly emitted, when treating that water is recycled near theoretical amount (water that generates when being NaOH and bis-phenol in the alkaline solution-S salify), upper strata dimethylbenzene begins clear, continue again to reflux 20 minutes, begin to steam dimethylbenzene then, along with steaming of dimethylbenzene, system temperature is increased to 220 ℃ of beginning constant temperature and carries out polymerization, continues after 6 hours, stopped reaction precipitates being poured in the 1000ml cold water under the polymerization mucus high temperature.Pulverize and filter with pulverizer then.Again the gained powder is steamed with 500ml cold water and boiled one hour and heat filtering, steam so repeatedly and boil 7～8 times, until using AgNO
3Solution checks that solution muddiness does not take place, shows till the no chlorion.
Made water content be lower than 0.5% in 12 hours 130 ℃ of oven dry the powder after refining and promptly obtain the PES resin, weighing gets the 114g polymkeric substance, and yield is 98%.Is η with DMA for the solvent one point method records viscosity
Ir=0.37, be fit to engineering plastics chlorine end group resin.Embodiment two
Change the monomer blends ratio among the embodiment one, get the two chlorine of 71.75g (0.25mol), 63.4g bis-phenol-S (0.2538mol) is that bis-phenol-S is excessive 1.5%, and other conditionally complete is with embodiment one, after refining the 113g polymkeric substance, use the similarity condition viscosimetric, must η
Ir=0.31, for being fit to coating terminal hydroxy group resin.Embodiment three
Change the ratio of components of embodiment one, the consumption of two chlorine changes 72.1g into, and other conditionally complete obtains the 114g polymkeric substance with embodiment one after making with extra care, and uses with the quadrat method viscosimetric, gets η
Ir=0.46, for being fit to ultra-filtration membrane manufacturing resin.Embodiment four
Embodiment one used dimethyl sulfone is changed into the dimethyl sulfone that reclaims.Other conditionally complete is identical with embodiment one, obtains the 113g polymkeric substance after making with extra care, and viscosimetric gets η
Ir=0.36, this shows that reclaiming dimethyl sulfone still can use repeatedly.Embodiment five
When embodiment one prepared polyethersulfone is handled, after each filtrate recovery is concentrated, water is steamed, concentrates, treat to place cooling when volume is close to 250ml, then constantly have the dimethyl sulfone crystallization to separate out, until the cool to room temperature after-filtration, the crystallization of gained dimethyl sulfone, dry back weighing 221g dimethyl sulfone, the rate of recovery about 80%, this dimethyl sulfone need not remake any refining polymer solvent that promptly can be used as.
Claims (3)
1, the present invention is a single stage method synthesizing polyether sulphone resin, it is characterized in that with the dimethyl sulfone being solvent, single stage method synthesizing polyether sulphone resin, and synthesize the various polyethersulfone resins that are suitable for different service requirementss by the adjusting of monomer ratio.
2, as right 1 described single stage method synthesizing polyether sulphone resin, it is characterized in that to regulate molecular weight of product by the excessive degree of monomer (between 1: 1～1.3).
3, as right 1 described single stage method synthesizing polyether sulphone resin, it is characterized in that boiling the recovery dimethyl sulfone that concentrates post crystallization can directly use again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99103164 CN1231302A (en) | 1999-03-24 | 1999-03-24 | One stage synthesizing polyether sulfone resin by using dimethyl sulfone as solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99103164 CN1231302A (en) | 1999-03-24 | 1999-03-24 | One stage synthesizing polyether sulfone resin by using dimethyl sulfone as solvent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1231302A true CN1231302A (en) | 1999-10-13 |
Family
ID=5271146
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99103164 Pending CN1231302A (en) | 1999-03-24 | 1999-03-24 | One stage synthesizing polyether sulfone resin by using dimethyl sulfone as solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1231302A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116342C (en) * | 2000-04-21 | 2003-07-30 | 吉林大学 | Synthesis of high solid content polyethersulphohe (PES) resin |
| CN103554498A (en) * | 2013-11-15 | 2014-02-05 | 威海洁瑞医用制品有限公司 | Polyether sulfone resin synthetic method |
| CN104271640A (en) * | 2012-05-11 | 2015-01-07 | 埃姆斯专利股份公司 | Method for the production of polysulfones, and polysulfones |
-
1999
- 1999-03-24 CN CN 99103164 patent/CN1231302A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116342C (en) * | 2000-04-21 | 2003-07-30 | 吉林大学 | Synthesis of high solid content polyethersulphohe (PES) resin |
| CN104271640A (en) * | 2012-05-11 | 2015-01-07 | 埃姆斯专利股份公司 | Method for the production of polysulfones, and polysulfones |
| CN104271640B (en) * | 2012-05-11 | 2016-12-21 | 埃姆斯专利股份公司 | Prepare method and the polysulfones of polysulfones |
| CN103554498A (en) * | 2013-11-15 | 2014-02-05 | 威海洁瑞医用制品有限公司 | Polyether sulfone resin synthetic method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105330861B (en) | A kind of high transparency polysulfone resin and preparation method thereof | |
| CN101704951A (en) | Method for preparing terpolymer of poly-diphenyl sulphone ether and polyether sulfone | |
| CN103724286B (en) | Method and system for coproducing tetrahydroxymethyl melamine and hexamethylol melamine | |
| CN115304752A (en) | Production process and system of poly (butylene adipate-terephthalate) | |
| CN109503540B (en) | Method for preparing epsilon-caprolactone and continuous production device thereof | |
| CN1231302A (en) | One stage synthesizing polyether sulfone resin by using dimethyl sulfone as solvent | |
| CN112898572A (en) | Preparation method of MQ resin with controllable molecular weight and hydroxyl content | |
| CN111072462A (en) | Bio-based bisphenol monomer, bio-based epoxy resin, composite material of bio-based bisphenol monomer and bio-based epoxy resin and preparation method of composite material | |
| CN101608015B (en) | Unsaturated polyester resin for electrical apparatus product moulding material and preparing method thereof | |
| CN107216608B (en) | A kind of compositions of thermosetting resin of highly corrosion resistant and its application | |
| CN104693428A (en) | Preparation method of high-molecular weight poly(butylene succinate) | |
| RU2059663C1 (en) | Method for production of carbamide-formaldehyde resin | |
| CN107955012A (en) | A kind of product preparative separation system and its processing method and purposes for being less than product and raw material for accessory substance boiling point | |
| CN119638561A (en) | Preparation method of aromatic diether dicarboxylic acid | |
| CN110330647B (en) | Remodelable shape memory bismaleimide resin and its application | |
| CN113698593A (en) | Composite material and preparation method thereof | |
| CN112961132A (en) | Method for preparing monochlorophthalic anhydride in micro-channel continuous flow reactor | |
| CN113321778B (en) | Thermosensitive film-forming resin for treatment-free CTP (computer to plate) plate and preparation method thereof | |
| CN105837791A (en) | Preparation method of hydantoin epoxy resin | |
| CN104262623A (en) | Reduced pressure rectification and dehydration technique of polyphenylene sulfide raw material (crystalline sodium sulfide) | |
| CN110872133B (en) | Novel process for preparing full water-soluble titanyl sulfate powder | |
| CN1345891A (en) | Method for controlling synthetic technological condition of producing polyphenyl-thioether | |
| CN108384187A (en) | A kind of preparation method of reinforced polyether ether ketone resin new material | |
| CN114736117A (en) | High-pressure hydrolysis recovery process for polylactic acid (PLA) residual liquid | |
| CN113336899A (en) | Unsaturated polyester resin for rapid pultrusion process and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |