CN105315453B - Polyglycerol based polyether polyol and preparation method thereof - Google Patents
Polyglycerol based polyether polyol and preparation method thereof Download PDFInfo
- Publication number
- CN105315453B CN105315453B CN201510834940.5A CN201510834940A CN105315453B CN 105315453 B CN105315453 B CN 105315453B CN 201510834940 A CN201510834940 A CN 201510834940A CN 105315453 B CN105315453 B CN 105315453B
- Authority
- CN
- China
- Prior art keywords
- polyether polyol
- parts
- based polyether
- polyglycerol based
- added
- 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 belongs to chemosynthesis technical field, and in particular to a kind of polyglycerol based polyether polyol and preparation method thereof.Polyglycerol based polyether polyol is made up of the raw material of following parts by weight：300 500 parts of initiator, 1,500 3000 parts of oxyalkylene, 5 10 parts of catalyst, 8 20 parts of nertralizer, 28 parts of adsorbent, 10 20 parts of composite assistant.Raw material of the present invention is easy to get, and pollution is few, and synthetic method is simple, easy to operate.
Description
Technical field
The invention belongs to chemosynthesis technical field, and in particular to a kind of polyglycerol based polyether polyol and its preparation side
Method.
Background technology
Presently commercially available Contents In Polyether Polyol often using sucrose, sorbierite, propane diols, glycerine etc. as initiator, its
The higher initiator of middle degree of functionality is mainly sucrose, sorbierite etc..Few products are directed to use with polyglycerol as main starting
System.
Polyglycerol is higher than the viscosity and boiling point of glycerine, and volatility and hygroscopicity are small, and moisture retention is good, and are improved emulsification
The characteristics of stability, therefore the fields such as cosmetics, fiber industry, plastics industry are frequently utilized for, but prepared as initiator poly-
The report of ether has no substantially.
It is used as being stripped in rubber using the Contents In Polyether Polyol that polyglycerol is prepared as main starting system
The main constituent of agent.The rubber inner pattern releasing agent applicable commonly used on the market at present often uses silicone emulsion class material, seldom has been reported that
It is related to polyglycerol base polyethers.Because polyglycerol has splendid moisture retention, the polyethers prepared by it as starting system is more
First alcohol product is then suitable as major constituent and prepares rubber inner pattern releasing agent applicable, uses at high temperature.
The content of the invention
It is an object of the invention to provide a kind of polyglycerol based polyether polyol, raw material is easy to get, pollution is lacked；The present invention is simultaneously
It is scientific and reasonable, simple and easy to apply, easy to operate there is provided the preparation method of polyglycerol based polyether polyol.
Polyglycerol based polyether polyol of the present invention, is made up of the raw material of following parts by weight：
Described initiator is the one or more in three polyglycereol, four polyglycereol or five polyglycereol.
Described oxyalkylene is the one or more in expoxy propane, oxirane or epoxy butane.
Described catalyst is potassium hydroxide.
Described nertralizer is phosphoric acid.
Described adsorbent is the mixture of magnesium silicate and alumina silicate, and the mass ratio of magnesium silicate and alumina silicate is 1:2-2:1.
Described composite assistant be without BHT liquid phenols complex type antioxidants, preferably Chic 3338 and Chic F96 (on
Hai Qike fluorine silicon materials Co., Ltd, commercially available prod) mixture, mass ratio is 1:2-2:1.
The preparation method of polyglycerol based polyether polyol of the present invention, step is as follows：
(1) feed：Initiator is added in autoclave, catalyst, nitrogen displacement is added；
(2) polymerisation：Add heat temperature raising after the oxyalkylene for accounting for oxyalkylene gross mass 5-6% to stir, pre-reaction,
Then proceed to be warming up to 100-120 DEG C, remaining oxyalkylene is added portionwise under pressurize, thick polyethers is obtained after post curing；
(3) post-process：Neutralization reaction is carried out with nertralizer to thick polyethers, adsorbent removing K is added+, and dehydrated under vacuum,
Filtering, adds composite assistant in obtained polyethers, produces colourless transparent liquid product.
Nitrogen displacement number of times described in step (1) is 3-5 times.
Pre-reaction temperature described in step (2) is 80-100 DEG C, and pre-reaction time is 2-3 hours, and dwell pressure is 0-
0.3Mpa, the post curing time is 4-6 hours.
Batch in batches described in step (2) is 8-10 batches.
Neutralization reaction temperature described in step (3) is 85-100 DEG C, and the neutralization reaction time is 1-1.5 hours.
The present invention compared with prior art, has the advantages that：
The present invention can obtain a kind of polyglycerol based polyether polyol product using polyglycerol as main starting system,
Such product occurs without relevant report on the market at present, and it is main that this kind of PPG is particularly suitable for rubber inner pattern releasing agent applicable
Component compounding use.Raw material of the present invention is easy to get, and pollution is few, and synthetic method is simple, easy to operate.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
It is being equipped with agitator, meter, heating temperature control device, cooling device (including external jacket and inner coil) and pressure
In the 5L autoclaves of sensor, four polyglycereol 362g, potassium hydroxide 5.5g are added, nitrogen displacement 5 times adds 135g oxirane
Heat temperature raising is stirred afterwards, and at 80-85 DEG C, pressure 0.25MPa reacts 2 hours.115 DEG C are warming up to afterwards, and Stress control exists
0.25MPa, is divided into 10 batches by remaining 2013g oxirane and adds successively, and charging is reacted after finishing, post curing 4 hours, Zhi Houjia
Enter phosphate aqueous solution nertralizer and neutralization reaction 1 hour is carried out at 100 DEG C, add magnesium silicate 1.5g and alumina silicate 1.5g, fully
Stirring is dehydrated, filtered under vacuo after 20 minutes, and antioxidant Chic 3338 is added in obtained polyethers：1.5g、Chic
F96：3.0g, stirs, and produces the final product that hydroxyl value is 195mgKOH/g.
Embodiment 2
It is being equipped with agitator, meter, heating temperature control device, cooling device (including external jacket and inner coil) and pressure
In the 5L autoclaves of sensor, three polyglycereol 100g, four polyglycereol 150g, five polyglycereol 110g, potassium hydroxide 6.5g, nitrogen are added
Gas is replaced 3 times, is added heat temperature raising after 190g expoxy propane and is stirred, at 80-85 DEG C, pressure 0.2MPa reacts 2 hours.Rise afterwards
Temperature is to 110 DEG C, and Stress control is divided into 8 batches in 0.3MPa, by remaining 2650g expoxy propane and added successively, and charging is reacted after finishing,
Post curing 5 hours, adds phosphate aqueous solution nertralizer and neutralization reaction 1 hour is carried out at 95 DEG C, add magnesium silicate 3.3g afterwards
With alumina silicate 2.3g, it is sufficiently stirred for after 20 minutes being dehydrated under vacuo, filters, antioxidant Chic is added in obtained polyethers
3338：5.0g、Chic F96：2.5g, stirs, and produces the final product that hydroxyl value is 125mgKOH/g.
Embodiment 3
It is being equipped with agitator, meter, heating temperature control device, cooling device (including external jacket and inner coil) and pressure
In the 5L autoclaves of sensor, four polyglycereol 350g, five polyglycereol 120g, potassium hydroxide 8g are added, nitrogen displacement 4 times is added
Heat temperature raising is stirred after 90g epoxy butanes, and at 80-85 DEG C, pressure 0.3MPa reacts 2 hours.115 DEG C, pressure are warming up to afterwards
Remaining 1558g expoxy propane is divided into 9 batches and added successively by control in 0.3MPa, and charging is reacted after finishing, post curing 6 hours, it
Phosphate aqueous solution nertralizer is added afterwards neutralization reaction 1 hour is carried out at 95 DEG C, add magnesium silicate 3g and alumina silicate 4.5g, fully
Stirring is dehydrated, filtered under vacuo after 20 minutes, and antioxidant Chic 3338 is added in obtained polyethers：3.0g、Chic
F96：3.0g, stirs, and produces the final product that hydroxyl value is 242mgKOH/g.
Claims (8)
1. a kind of polyglycerol based polyether polyol, it is characterised in that be made up of the raw material of following parts by weight：
300-500 parts of initiator
1500-3000 parts of oxyalkylene
5-10 parts of catalyst
8-20 parts of nertralizer
2-8 parts of adsorbent
10-20 parts of composite assistant；
Described initiator is the one or more in three polyglycereol, four polyglycereol or five polyglycereol；
Described composite assistant is without BHT liquid phenols complex type antioxidants.
2. polyglycerol based polyether polyol according to claim 1, it is characterised in that described oxyalkylene is epoxy
One or more in propane, oxirane or epoxy butane.
3. polyglycerol based polyether polyol according to claim 1, it is characterised in that described catalyst is hydroxide
Potassium.
4. polyglycerol based polyether polyol according to claim 1, it is characterised in that described nertralizer is phosphoric acid.
5. polyglycerol based polyether polyol according to claim 1, it is characterised in that described adsorbent is magnesium silicate
With the mixture of alumina silicate, the mass ratio of magnesium silicate and alumina silicate is 1:2-2:1.
6. a kind of preparation method of any described polyglycerol based polyether polyols of claim 1-5, it is characterised in that step
It is as follows：
（1）Charging：Initiator is added in autoclave, catalyst, nitrogen displacement is added；
（2）Polymerisation：Add heat temperature raising after the oxyalkylene for accounting for oxyalkylene gross mass 5-6% to stir, pre-reaction, then
100-120 DEG C is continuously heating to, remaining oxyalkylene is added portionwise under pressurize, thick polyethers is obtained after post curing；
（3）Post processing：Neutralization reaction is carried out with nertralizer to thick polyethers, adsorbent removing K is added+, and dehydrated under vacuum, filtering,
Composite assistant is added in obtained polyethers, colourless transparent liquid product is produced.
7. the preparation method of polyglycerol based polyether polyol according to claim 6, it is characterised in that step（2）Middle institute
The pre-reaction temperature stated is 80-100 DEG C, and pre-reaction time is 2-3 hours, and dwell pressure is 0-0.3MPa, and the post curing time is
4-6 hours.
8. the preparation method of polyglycerol based polyether polyol according to claim 6, it is characterised in that step（3）Middle institute
The neutralization reaction temperature stated is 85-100 DEG C, and the neutralization reaction time is 1-1.5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510834940.5A CN105315453B (en) | 2015-11-25 | 2015-11-25 | Polyglycerol based polyether polyol and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510834940.5A CN105315453B (en) | 2015-11-25 | 2015-11-25 | Polyglycerol based polyether polyol and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105315453A CN105315453A (en) | 2016-02-10 |
| CN105315453B true CN105315453B (en) | 2017-07-14 |
Family
ID=55243833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510834940.5A Active CN105315453B (en) | 2015-11-25 | 2015-11-25 | Polyglycerol based polyether polyol and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105315453B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860051A (en) * | 2016-06-29 | 2016-08-17 | 句容宁武新材料股份有限公司 | Method for preparing low-odor polyether for polyurethane foam and application of prepared products |
| CN106117537A (en) * | 2016-06-29 | 2016-11-16 | 句容宁武新材料股份有限公司 | The polyurethane foam preparation method of low volatile matter polyethers and the application of prepared product |
| CN106243338A (en) * | 2016-07-30 | 2016-12-21 | 淄博德信联邦化学工业有限公司 | The preparation method of the polyether polyol of low abnormal smells from the patient low volatile |
| CN108059717B (en) * | 2016-11-09 | 2021-05-11 | 中国石油化工股份有限公司 | Refining method and application of low-odor polyether polyol |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362505A (en) * | 2000-12-25 | 2002-08-07 | 资生堂贺妮健工业株式会社 | Transparent bar-type soap composition |
| CN100999574A (en) * | 2006-11-28 | 2007-07-18 | 王伟松 | Synthesizing process of glycerin polyether |
| CN101084297A (en) * | 2004-12-17 | 2007-12-05 | 宝洁公司 | Hydrophobically modified polyols for improved hydrophobic soil cleaning |
| CN101376089A (en) * | 2008-09-28 | 2009-03-04 | 亚邦(福建)生化有限公司 | Method for preparing foam killer |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5617599B2 (en) * | 2010-12-17 | 2014-11-05 | 日油株式会社 | Sanitary paper softener |
-
2015
- 2015-11-25 CN CN201510834940.5A patent/CN105315453B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362505A (en) * | 2000-12-25 | 2002-08-07 | 资生堂贺妮健工业株式会社 | Transparent bar-type soap composition |
| CN101084297A (en) * | 2004-12-17 | 2007-12-05 | 宝洁公司 | Hydrophobically modified polyols for improved hydrophobic soil cleaning |
| CN100999574A (en) * | 2006-11-28 | 2007-07-18 | 王伟松 | Synthesizing process of glycerin polyether |
| CN101376089A (en) * | 2008-09-28 | 2009-03-04 | 亚邦(福建)生化有限公司 | Method for preparing foam killer |
Non-Patent Citations (1)
| Title |
|---|
| 一种新型软泡聚醚多元醇的研制;李兆星等;《精细与专用化学品》;20060921;第14卷(第18期);第18-20页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105315453A (en) | 2016-02-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105315453B (en) | Polyglycerol based polyether polyol and preparation method thereof | |
| Poutrel et al. | Dicarboxylic acid-epoxy vitrimers: influence of the off-stoichiometric acid content on cure reactions and thermo-mechanical properties | |
| CN110885435B (en) | Process for preparing high functionality polyether polyols | |
| CN106810682A (en) | The preparation method of rigid-foam polyether polyol | |
| DE202009019002U1 (en) | New alkoxysilyl-bearing polyether alcohols | |
| CN107573500A (en) | A kind of preparation method of high-purity polyether-ether-ketone resin | |
| CN106750241B (en) | The preparation method of the allyl polyether polyalcohol of secondary hydroxyl sealing end | |
| CN105237759B (en) | Tensile elasticity body PPG high and preparation method thereof | |
| CN107200837A (en) | A kind of method that utilization dmc catalyst circulation prepares PPG | |
| CN103665885A (en) | High-tear strength silicone rubber and preparation method thereof | |
| CN105801862A (en) | Preparation method of low-viscosity high-strength addition type liquid silicone rubber | |
| CN104774312A (en) | Resin with mixing and solidification functions and synthetic method thereof | |
| CN103131181A (en) | Toughened cyanate resin and preparation method thereof | |
| CN104725590B (en) | A kind of low modulus water-base polyurethane material | |
| CN101035837B (en) | Process for the preparation of polymeric hydroxyalkyl terminated polysulphides | |
| CN105131254A (en) | Synthesis method for high-flexibility and high-hydrophobicity epoxy resin | |
| CN102352032B (en) | Method for preparing high purity polysorbate 80 through esterification of oleic acid and mixture of respectively etherified starting materials | |
| CN114163598A (en) | Self-repairing polyurethane derived from bio-based polyol and preparation method thereof | |
| CN107057051A (en) | High activity rigid foam polyether polyatomic alcohol and preparation method thereof | |
| CN104592480A (en) | Preparation method of polyurethane modified polysulfide rubber | |
| CN105461915A (en) | Polyester-polyether polyol for microporous PU (polyurethane) shoe sole and preparation method of polyester-polyether polyol as well as PU shoe sole stock solution prepared from polyester-polyether polyol and preparation method of PU shoe sole stock solution | |
| CN111072947A (en) | Preparation method of low-unsaturation degree, ultrahigh molecular weight and low viscosity polyether polyol | |
| CN109880083A (en) | A kind of impact resistance amide hydridization polyester and preparation method thereof | |
| CN111718485A (en) | Viscosity of 475mm2/s～525mm2Production method of medicinal dimethyl silicone oil/s | |
| CN108530596B (en) | Triazole bond crosslinked poly-nitrogen glycidyl ether and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: Linzi District of Shandong Province Jin Shan Zhen Feng Guan Lu 255400 Zibo City No. 58 Applicant after: SHANDONG INOV NEW MATERIAL CO., LTD. Address before: 255400 Shandong Province, Zibo city Linzi District South East Nanshan Road West five by ethylene Applicant before: SHANDONG INOV NEW MATERIAL CO., LTD. |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |