CN100549065C - Synthesis method of acetyl terminated allyl alcohol polyether - Google Patents
Synthesis method of acetyl terminated allyl alcohol polyether Download PDFInfo
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- CN100549065C CN100549065C CNB2007100701571A CN200710070157A CN100549065C CN 100549065 C CN100549065 C CN 100549065C CN B2007100701571 A CNB2007100701571 A CN B2007100701571A CN 200710070157 A CN200710070157 A CN 200710070157A CN 100549065 C CN100549065 C CN 100549065C
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- CN
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- Prior art keywords
- allyl alcohol
- alcohol polyether
- polyether
- synthetic method
- acetyl blocked
- Prior art date
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- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229920000570 polyether Polymers 0.000 title claims abstract description 56
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 44
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 title claims abstract 12
- 238000001308 synthesis method Methods 0.000 title 1
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 238000010189 synthetic method Methods 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 239000011552 falling film Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003463 adsorbent Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000000605 extraction Methods 0.000 claims description 5
- 230000003311 flocculating effect Effects 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002594 sorbent Substances 0.000 claims description 2
- 230000005587 bubbling Effects 0.000 abstract description 4
- 238000009833 condensation Methods 0.000 abstract description 4
- 230000005494 condensation Effects 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 3
- 238000006297 dehydration reaction Methods 0.000 abstract description 3
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- 229910001414 potassium ion Inorganic materials 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 14
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000012661 block copolymerization Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
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- Polyethers (AREA)
Abstract
A synthetic method of acetyl terminated allyl alcohol polyether, belong to the synthetic technical field of terminated polyether, take allyl alcohol polyether and acetic anhydride as raw materials to carry on the condensation reflux reaction, after the condensation reflux reaction, remove most of acid through nitrogen bubbling way under the vacuumized condition first, remove surplus acetic acid and acetic anhydride under the high vacuum condition through the falling film evaporator, then add water and polyether adsorbent to absorb, add filter aid and carry on the vacuum dehydration and filtration to make acetyl terminated allyl alcohol polyether; the mol ratio of the allyl alcohol polyether to the acetic anhydride can be 1: 2.0-2.5. According to the invention, most of acetic acid and acetic anhydride are removed by bubbling nitrogen under a vacuum pumping condition, then the rest of acetic acid and acetic anhydride are removed by a falling film evaporator under a high vacuum condition, and the acetyl-terminated allyl alcohol polyether is prepared by processes of potassium and sodium ion adsorption and the like.
Description
Technical field
The present invention relates to a kind of synthetic method of acetyl blocked allyl alcohol polyether, belong to the synthesis technical field of end capped polyether.
Background technology
Acetyl blocked allyl alcohol polyether is meant the polyethers that the hydrogen on the allyl alcohol polyether terminal hydroxyl is replaced by ethanoyl.Acetyl blocked allyl alcohol polyether also has many special propertys except that the character with allyl alcohol polyether, for example the polyether foam behind the end-blocking is low, and lipophilicity is strong, and yield point is low, and viscosity character such as diminish is applicable to fields such as synthesizing polyether modified organic silicon.At present, acetyl blocked allyl alcohol polyether the rarely seen report of synthesis technique.
Summary of the invention
It is reasonable to the purpose of this invention is to provide a kind of technology, simple to operate, has the synthetic method of the acetyl blocked allyl alcohol polyether of better use properties.
The expression formula of acetyl blocked allyl alcohol polyether is:
In the formula: m+n=3～100
The allyl alcohol polyether segment is homopolymerization or block copolymerization.
The present invention is the synthetic method of acetyl blocked allyl alcohol polyether; with allyl alcohol polyether and diacetyl oxide is that raw material carries out the condensing reflux reaction; after it is characterized in that the condensing reflux reaction; deviate from most of acid by nitrogen bubble mode under the condition of vacuumizing earlier; under high vacuum condition, deviate from residual acetic acid and diacetyl oxide by falling-film evaporator again; add water and polyethers adsorbents adsorb then, add flocculating aids and carry out vacuum hydro-extraction and filter and to make acetyl blocked allyl alcohol polyether.
The mol ratio of described allyl alcohol polyether and diacetyl oxide can be 1: 2.0～and 2.5.
The temperature of reaction of described condensing reflux reaction can be 130 ℃～140 ℃, and the reaction times is 2.0～2.5 hours.
Described nitrogen can be common bottled nitrogen, and its feeding amount can adjust accordingly according to described vacuum tightness.
Temperature in the described nitrogen bubble deacidification process can be 120 ℃～130 ℃, and vacuum tightness is-0.080MPa～-0.090MPa, the time is 2.0～3.0 hours.
Temperature under the described falling-film evaporator high vacuum condition in the deacidification process can be 100 ℃～120 ℃, and vacuum tightness is≤100Pa that the time is 1.0～2.0 hours.
The add-on of water and polyethers sorbent material is 1.5%～3.0% of an allyl alcohol polyether weight in the described polyethers adsorbents adsorb operation, and adsorption temp is 60 ℃～70 ℃, and the time is 30～50 minutes.
The add-on of flocculating aids is 0.5%～1.0% in the described vacuum hydro-extraction operation, and temperature is 90 ℃～100 ℃, vacuum tightness is-and 0.093MPa～-0.098MPa, the time is 1.0～1.5 hours.
Temperature in the described filtration operation can be 55 ℃～70 ℃.
Advantage of the present invention is to deviate from most acetate and diacetyl oxide by nitrogen bubble under the condition of vacuumizing; deviate from residual acetic acid and diacetyl oxide by falling-film evaporator under high vacuum condition then, processes such as k adsorption, sodium ion are produced acetyl blocked allyl alcohol polyether.Simultaneously the add-on and the proportioning of allyl alcohol polyether and diacetyl oxide in the condensing reflux reaction are rationally adjusted, temperature of reaction and time in the operations such as condensing reflux reaction, polyethers adsorbents adsorb, vacuum hydro-extraction are optimized selection, technology is reasonable, and is simple to operate.By the acetyl blocked allyl alcohol polyether that the present invention makes, end-blocking rate height, steady quality, potassium, sodium ions content is low, reactive behavior good, is applicable to fields such as synthesizing polyether modified organic silicon.
Embodiment
In an embodiment, the end-blocking rate is defined as:
Embodiment 1:
Add 1800 parts of allyl alcohol random polyethers (M=1500) in reactor, 245 parts of diacetyl oxides connect condensation reflux unit, are warming up to 130 ℃～140 ℃, back flow reaction 2.5 hours.Connect water distilling apparatus, adjust nitrogen feeding amount, make vacuum tightness be-0.080MPa～-0.085MPa, bubbling depickling 2.5 hours.Be cooled to 70 ℃; change falling-film evaporator over to; depickling is 1.5 hours under the condition of vacuum tightness≤100Pa; being cooled to 70 ℃, adding 30 parts of 37.5 parts of water, polyethers treating adsorbents, is to stir 30 minutes under 60 ℃～70 ℃ conditions in temperature; add 14 parts of super-cells then; vacuum tightness for-0.095MPa～-0.097MPa, temperature are dehydration 1 hour under 90 ℃～100 ℃ the condition, be cooled to 60 ℃ filter the acetyl blocked allyl alcohol atactic polyether, the end-blocking rate is 98%.
Embodiment 2:
Add 1600 parts of allyl alcohol random polyethers (M=4000) in reactor, 102 parts of diacetyl oxides connect condensation reflux unit, are warming up to 130 ℃～140 ℃, back flow reaction 2.5 hours.Connect water distilling apparatus, adjust nitrogen feeding amount, make vacuum tightness be-0.085MPa～-0.090MPa, bubbling depickling 3.0 hours.Be cooled to 70 ℃; change falling-film evaporator over to; depickling is 2.0 hours under the condition of vacuum tightness≤100Pa; after be cooled to 70 ℃, add 48 parts of 48 parts of water, polyethers treating adsorbents, be to stir under 60 ℃～70 ℃ conditions 50 minutes in temperature; add 16 parts of super-cells then; vacuum tightness for-0.095MPa～-0.097MPa, temperature are dehydration 1.5 hours under 90 ℃～100 ℃ the condition, after be cooled to 60 ℃ filter the acetyl blocked allyl alcohol atactic polyether, the end-blocking rate is 95%.
Claims (8)
1, a kind of synthetic method of acetyl blocked allyl alcohol polyether, with allyl alcohol polyether and diacetyl oxide is that raw material carries out the condensing reflux reaction, after it is characterized in that the condensing reflux reaction, deviate from most of acid by nitrogen bubble mode under the condition of vacuumizing earlier, under high vacuum condition, deviate from residual acetic acid and diacetyl oxide by falling-film evaporator again, add water and polyethers adsorbents adsorb then, add that flocculating aids carries out vacuum hydro-extraction and filtration makes acetyl blocked allyl alcohol polyether; Temperature in the described nitrogen bubble deacidification process is 120 ℃～130 ℃, vacuum tightness is-and 0.080MPa～-0.090MPa, the time is 2.0～3.0 hours.
2, by the synthetic method of the described acetyl blocked allyl alcohol polyether of claim 1, the mol ratio that it is characterized in that described allyl alcohol polyether and diacetyl oxide is 1: 2.0～2.5.
3, by the synthetic method of the described acetyl blocked allyl alcohol polyether of claim 1, it is characterized in that described condensing reflux temperature of reaction is 130 ℃～140 ℃, the reaction times is 2.0～2.5 hours.
4, by the synthetic method of the described acetyl blocked allyl alcohol polyether of claim 1, it is characterized in that described nitrogen is common bottled nitrogen.
5, by the synthetic method of the described acetyl blocked allyl alcohol polyether of claim 1, it is characterized in that the temperature in the deacidification process is 100 ℃～120 ℃ under the described falling-film evaporator high vacuum condition, vacuum tightness is≤100Pa that the time is 1.0～2.0 hours.
6, press the synthetic method of the described acetyl blocked allyl alcohol polyether of claim 1; it is characterized in that the add-on of water and polyethers sorbent material is 1.5%～3.0% of an allyl alcohol polyether weight in the described polyethers adsorbents adsorb operation; adsorption temp is 60 ℃～70 ℃, and the time is 30～50 minutes.
7, press the synthetic method of the described acetyl blocked allyl alcohol polyether of claim 1; the add-on that it is characterized in that flocculating aids in the described vacuum hydro-extraction operation is 0.5%～1.0%; temperature is 90 ℃～100 ℃, vacuum tightness is-and 0.093MPa～-0.098MPa, the time is 1.0～1.5 hours.
8, by the synthetic method of the described acetyl blocked allyl alcohol polyether of claim 1, it is characterized in that the temperature in the described filtration operation is 55 ℃～70 ℃.
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| CNB2007100701571A CN100549065C (en) | 2007-07-24 | 2007-07-24 | Synthesis method of acetyl terminated allyl alcohol polyether |
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| CNB2007100701571A CN100549065C (en) | 2007-07-24 | 2007-07-24 | Synthesis method of acetyl terminated allyl alcohol polyether |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101497689B (en) * | 2008-12-30 | 2011-04-20 | 浙江皇马科技股份有限公司 | Preparation of acetyl end capping allyl alcohol polyether |
| CN102911352B (en) * | 2012-10-25 | 2014-11-05 | 浙江皇马科技股份有限公司 | Preparation method of low-molecular-weight acetyl-terminated allyl alcohol polyether |
| CN106279668B (en) * | 2016-08-19 | 2018-03-09 | 浙江皇马科技股份有限公司 | A kind of acetyl blocked polyethers and preparation method thereof |
| CN106633030B (en) * | 2016-12-20 | 2020-05-22 | 江苏钟山化工有限公司 | Preparation method of high molecular weight narrow distribution esterification terminated allyl alcohol polyether |
| CN113234218B (en) * | 2021-04-26 | 2023-06-30 | 南京威尔生物科技有限公司 | Preparation method of acetyl-terminated allyl alcohol polyether |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1302457A2 (en) * | 2001-10-16 | 2003-04-16 | Takemoto Yushi Kabushiki Kaisha | Method of producing allyletherester monomers and cement dispersants |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1302457A2 (en) * | 2001-10-16 | 2003-04-16 | Takemoto Yushi Kabushiki Kaisha | Method of producing allyletherester monomers and cement dispersants |
| CN1412175A (en) * | 2001-10-16 | 2003-04-23 | 竹本油脂株式会社 | Method for producing allyl ether ester monomer and cement dispersant |
| CN1807334A (en) * | 2001-10-16 | 2006-07-26 | 竹本油脂株式会社 | cement dispersant |
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Owner name: ZHEJIANG HUANGMA TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: WANG WEISONG Effective date: 20100601 |
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Free format text: CORRECT: ADDRESS; FROM: 312300 ZHEJIANG HUANGMA CHEMICAL INDUSTRY GROUP CO., LTD., INDUSTRIAL NEW ZONE, ZHANG TOWN, SHANGYU CITY, ZHEJIANG PROVINCE TO: 312363 ZHEJIANG HUANGMA TECHNOLOGY CO., LTD., INDUSTRIAL NEW ZONE, ZHANG TOWN, SHANGYU CITY, ZHEJIANG PROVINCE |
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Effective date of registration: 20100601 Address after: 312363, Shangyu Town, Zhejiang Province Industrial Zone, Zhejiang Real Madrid Polytron Technologies Inc Patentee after: Zhejiang Huangma Technology Co., Ltd. Address before: 312300, Shangyu, Zhejiang Province town industrial zone, Zhejiang Real Madrid Chemical Group Co., Ltd. Patentee before: Wang Weisong |