CN106317400A - Synthesis method of gamma type silane-terminated polyether - Google Patents
Synthesis method of gamma type silane-terminated polyether Download PDFInfo
- Publication number
- CN106317400A CN106317400A CN201610767346.3A CN201610767346A CN106317400A CN 106317400 A CN106317400 A CN 106317400A CN 201610767346 A CN201610767346 A CN 201610767346A CN 106317400 A CN106317400 A CN 106317400A
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- China
- Prior art keywords
- type silane
- terminated polyether
- polyether
- hydroxyl
- terminated
- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/71—Monoisocyanates or monoisothiocyanates
- C08G18/718—Monoisocyanates or monoisothiocyanates containing silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/336—Polymers modified by chemical after-treatment with organic compounds containing silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/50—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing nitrogen, e.g. polyetheramines or Jeffamines(r)
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polyethers (AREA)
Abstract
The invention provides a synthesis method of gamma type silane-terminated polyether. The synthesis method comprises following steps: hydroxyl-terminated polyether glycol with appropriate molecular weight is selected, isocyanatopropyltrimethoxysilane or isocyanatopropyltriethoxysilane is added under the action of a catalyst, a mixture is heated to 60-130 DEG C and reacts for 60-180 min, and gamma type silane-terminated polyether is obtained finally. According to the synthesis method of gamma type silane-terminated polyether, introduction of high-price isocyanate silane which is inconvenient to produce is avoided; existence of hydroxyl is harmful to stability of a follow-up formula, and by means of the two-step reaction, hydroxyl on polyether molecular chains is removed more completely.
Description
Technical field
The invention belongs to the synthesis technical field of chemical products, particularly to the synthetic method of γ type silane-terminated polyether.
Background technology
The method producing silane end capped polyurethane in the market has multiple, however it is necessary that introduction price is high and produces not
Isocyanato silanes easily, and the hydroxyl on the pfpe molecule chain in reactions steps cannot eliminate thoroughly, and hydroxyl
Existence unfavorable to the stability of later stage formula.
Summary of the invention
Goal of the invention: the technical problem to be solved is to provide the synthetic method of γ type silane-terminated polyether.
Technical scheme: the present invention provides the γ synthetic method of type silane-terminated polyether, comprises the following steps: select suitable point
Son amount hydroxy-end capped polyether polyol, under the effect of catalyst, add NCO propyl trimethoxy silicane or
Person's NCO propyl-triethoxysilicane, is heated to 60～130 DEG C and carries out reacting 60～180 minutes, finally give γ type
Silante terminated polyethers.Wherein, NCO propyl trimethoxy silicane and NCO propyl-triethoxysilicane are equal
For commercially available prod.
Synthetic reaction formula is specific as follows:
R is first
Epoxide or ethyoxyl.
Wherein, above-mentioned polyether polyol molecular weight is 3000～10000.
Wherein, while hydroxy-end capped or hydroxy-end capped in above-mentioned polyether polyol, side chain also contains hydroxyl.
Wherein, the hydroxyl of above-mentioned polyether polyol and NCO propyl trimethoxy silicane or NCO third
The ratio of-the NCO of ethyl triethoxy silicane alkane is 2:1～1:2.
Wherein, above-mentioned catalyst is organic titanium.
Present invention additionally comprises the γ type silane-terminated polyether of above-mentioned legal manner synthesis.
Present invention additionally comprises the application in terms of preparation chemical products of the above-mentioned γ type silane-terminated polyether.
Beneficial effect: relative to prior art, the present invention possesses advantages below:
1, the two-step reaction hydroxyl to eliminating on pfpe molecule chain is more thorough, and later stage formula is stablized by the existence of hydroxyl
Property is unfavorable；
2, reactions steps of the present invention need not add the environmentally harmful catalyst such as organotin or Organic leadP；Therefore this is anti-
Response environment does not pollute, and belongs to environmentally friendly chemical reaction.
3, after the polymer that present invention reaction obtains is by carrying out performance test after adding aminopropyl trimethoxysilane, respectively
The performance of aspect is superior to the product bought on the market.
Detailed description of the invention
According to following embodiment, the present invention be may be better understood.But, as it will be easily appreciated by one skilled in the art that reality
Execute concrete material proportion, process conditions and result thereof described by example and be merely to illustrate the present invention, and should also will not limit
The present invention described in detail in claims processed.
The preparation of embodiment 1 γ type silane-terminated polyether
Choose poly(propylene oxide) PPG8000 that end is hydroxyl, reaction bulb adds this polyether polyol, is subsequently adding
NCO propyl trimethoxy silicane, adds catalyst organic titanium, reacts 60 minutes at 90 DEG C, is cooled to room temperature
Obtain polymer 1.Hydroxyl is 2:1 with the ratio of-NCO of NCO propyl trimethoxy silicane.
Polymer 1 viscosity: 3500～5000mPa.s
Polymer 1 color: colourless or light yellow transparent liquid
In polymer 1, add aminopropyl trimethoxysilane 3%, test and obtain following performance:
Surface drying time: 14～20 minutes；
24 hours curing depths: > 2mm
Interiors of products bubble-free after solidification.
The preparation of embodiment 2 γ type silane-terminated polyether
Essentially the same with embodiment 1, except that, choose poly(propylene oxide) PPG3000 that end is hydroxyl, in reaction
Add this polyether polyol in Ping, be subsequently adding NCO propyl-triethoxysilicane, hydroxyl and NCO propyl group
The mol ratio of-the NCO of triethoxysilane is 1:2, adds catalyst organic titanium, reacts 180 minutes at 60 DEG C, is cooled to room
Temperature i.e. can get polymer 2.
Polymer 2 viscosity: 3500～5000mPa.s
Polymer 2 color: colourless or light yellow transparent liquid
In polymer 2, add aminopropyl trimethoxysilane 3%, test and obtain following performance:
Surface drying time: 14～20 minutes；
24 hours curing depths: > 2mm
Interiors of products bubble-free after solidification.
The preparation of embodiment 3 γ type silane-terminated polyether
Essentially the same with embodiment 1, except that, choose poly(propylene oxide) PPG6500 that end is hydroxyl, in reaction
Add this polyether polyol in Ping, be subsequently adding NCO propyl-triethoxysilicane, hydroxyl and NCO propyl group
The weight ratio of-the NCO of triethoxysilane is 1:2, adds catalyst organic titanium, reacts 180 minutes at 65 DEG C, is cooled to room
Temperature i.e. can get polymer 3.
Polymer 3 viscosity: 3500～5000mPa.s
Polymer 3 color: colourless or light yellow transparent liquid
In polymer 3, add aminopropyl trimethoxysilane 3%, test and obtain following performance:
Surface drying time: 14～20 minutes；
24 hours curing depths: > 2mm
Interiors of products bubble-free after solidification.
The preparation of embodiment 4 γ type silane-terminated polyether
Essentially the same with embodiment 1, except that, change the molecular weight of PPG into 12000, prepare polymer 4.
Polymer 4 viscosity: 3500～5000mPa.s
Polymer 4 color: colourless or light yellow transparent liquid
In polymer 4, add aminopropyl trimethoxysilane 3%, test and obtain following performance:
Surface drying time: 14～20 minutes；
24 hours curing depths: > 2mm
Interiors of products bubble-free after solidification.
Experimental example
Polymer 1 that embodiment 1～4 is prepared, polymer 2, polymer 3, polymer 4 and buy on the market
Common α type silicone modified polymers, organosilicon, organosilicon modified polyether have carried out performance test contrast:
Claims (7)
1. the synthetic method of γ type silane-terminated polyether, it is characterised in that comprise the following steps: select the hydroxyl of suitable molecular weight
The polyether polyol of end-blocking, under the effect of catalyst, adds NCO propyl trimethoxy silicane or isocyanates
Base propyl-triethoxysilicane, is heated to 60 ~ 130 DEG C and carries out reacting 60 ~ 180 minutes, finally gives Silante terminated the gathering of γ type
Ether.
The synthetic method of γ type silane-terminated polyether the most according to claim 1, it is characterised in that described polyether polyol
Molecular weight is 3000 ~ 10000.
The synthetic method of γ type silane-terminated polyether the most according to claim 1, it is characterised in that described polyether polyol
In hydroxy-end capped or hydroxy-end capped while side chain also contain hydroxyl.
The synthetic method of γ type silane-terminated polyether the most according to claim 1, it is characterised in that described polyether polyol
Hydroxyl and NCO propyl trimethoxy silicane or the ratio of-NCO of NCO propyl-triethoxysilicane
For 2:1 ~ 1:2.
The synthetic method of γ type silane-terminated polyether the most according to claim 1, it is characterised in that described catalyst is for having
Machine titanium.
6. the γ type silane-terminated polyether of the legal manner synthesis described in claim 1 ~ 5.
7. the application in terms of preparation chemical products of the γ type silane-terminated polyether described in claim 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610767346.3A CN106317400A (en) | 2016-08-30 | 2016-08-30 | Synthesis method of gamma type silane-terminated polyether |
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| CN201610767346.3A CN106317400A (en) | 2016-08-30 | 2016-08-30 | Synthesis method of gamma type silane-terminated polyether |
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| CN201610767346.3A Pending CN106317400A (en) | 2016-08-30 | 2016-08-30 | Synthesis method of gamma type silane-terminated polyether |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007169495A (en) * | 2005-12-22 | 2007-07-05 | Momentive Performance Materials Japan Kk | Room-temperature curable silicon group-containing polymer composition |
| JP2010150382A (en) * | 2008-12-25 | 2010-07-08 | Asahi Glass Co Ltd | Curable composition |
| CN102482486A (en) * | 2009-08-17 | 2012-05-30 | 旭硝子株式会社 | Curable composition |
-
2016
- 2016-08-30 CN CN201610767346.3A patent/CN106317400A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007169495A (en) * | 2005-12-22 | 2007-07-05 | Momentive Performance Materials Japan Kk | Room-temperature curable silicon group-containing polymer composition |
| JP2010150382A (en) * | 2008-12-25 | 2010-07-08 | Asahi Glass Co Ltd | Curable composition |
| CN102482486A (en) * | 2009-08-17 | 2012-05-30 | 旭硝子株式会社 | Curable composition |
Non-Patent Citations (4)
| Title |
|---|
| 中国大百科全书总编辑委员会编: "《中国大百科全书化学Ι》", 28 February 1983, 中国大百科全书出版社 * |
| 刘益军编著: "《聚氨酯树脂及其应用》", 30 January 2012, 化学工业出版社 * |
| 徐祖顺等编著: "《织物用胶黏剂及其粘接技术》", 31 August 2004, 化学工业出版社材料科学与工程出版中心 * |
| 朱吕民等编著: "《聚氨酯泡沫塑料 第三版》", 31 January 2005, 化学工业出版社材料科学与工程出版中心 * |
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Application publication date: 20170111 |
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