CN100588671C - Synthesizing process of butylol polyether - Google Patents
Synthesizing process of butylol polyether Download PDFInfo
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- CN100588671C CN100588671C CN200610154860A CN200610154860A CN100588671C CN 100588671 C CN100588671 C CN 100588671C CN 200610154860 A CN200610154860 A CN 200610154860A CN 200610154860 A CN200610154860 A CN 200610154860A CN 100588671 C CN100588671 C CN 100588671C
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Abstract
The process of synthesizing polybutanol ether belongs to the field of polyether synthesis technology. Polybutanol ether is prepared through reaction with butanol or polybutanol ether of low molecularweight as initial material, epoxy propane or its mixture with epoxy ethane or epoxy butane as chain extender, and multimetallic cyanide of Co, Zn, Pb, etc as catalyst and at 90-160 deg.c. The amount of the catalyst is 0.002-0.015 wt% of ultimate product. The present invention has reasonable technological process, fast reaction speed, shortened reaction period, no need of post-treatment and other advantages, and the prepared polyether has effectively increased molecular weight and lowered unsaturation degree.
Description
Technical field
The present invention relates to a kind of synthetic method of butylol polyether, belong to the synthesis technical field of polyethers.
Background technology
As everyone knows, make catalyzer with highly basic, the mixture that adds propylene oxide or propylene oxide and oxyethane or butylene oxide ring, the preparation butylol polyether, low-carbon alcohol polyethers particularly: as methyl alcohol, ethanol, propyl alcohol, butanols etc., general molecular weight all is no more than 4000, and degree of unsaturation is again more than 0.02, product second-rate, and the production cycle is long.
Summary of the invention
It is reasonable to the purpose of this invention is to provide a kind of technology, can effectively improve the molecular weight of polyethers, reduces degree of unsaturation, shortens the synthetic method of the butylol polyether of production cycle.
The present invention is the synthetic method of butylol polyether, with butanols or lower molecular weight butylol polyether is initiator, the mixture of propylene oxide or propylene oxide and oxyethane or butylene oxide ring is a chain extension agent, it is characterized in that to contain Co, Zn, the multi-metal cyanide of metal ions such as Pb (MMC) is a catalyzer, in temperature is to react under 90～160 ℃ the condition, makes butylol polyether.
The add-on of described catalyzer can be 0.002～0.015% of the butylol polyether the finished product weight percent that makes.
The molecular weight of the described butylol polyether that makes and corresponding degree of unsaturation are respectively: molecular weight is that 300～1000 o'clock degrees of unsaturation are 0.01～0.0005, molecular weight is that 1000～2000 o'clock degrees of unsaturation are 0.0015～0.0006, molecular weight is that 2000～5000 o'clock degrees of unsaturation are 0.02～0.0006, and molecular weight is that 5000～25000 o'clock degrees of unsaturation are 0.05～0.001.
It is catalyzer that the present invention adopts the multi-metal cyanide (MMC) that contains metal ions such as Co, Zn, Pb, solved in the prior art when the preparation butylol polyether molecular weight and done not highly, and need carry out aftertreatment with the butylol polyether that highly basic makes and remove the metal ion of the inside (as K
+, Na
+) problem, have speed of response fast, with short production cycle, needn't carry out outstanding advantage and positively effect such as postprocessing working procedures, can effectively improve the molecular weight of polyethers, reduce degree of unsaturation, shorten the production cycle.
Embodiment
The preparation of reactor before implementing: with distilled water the 2.5L autoclave is washed several times earlier, till clean, dried reactor, standby after being cooled to 25 ℃.
Embodiment 1:
In reactor, add butanols 200g, contain multi-metal cyanide (MMC) the catalyzer 0.075g of metal ions such as Co, Zn, Pb, displacement N
2Heat up after three times, temperature to 125 ℃, (add 30g earlier, pressure is 0.3～0.9Mpa to add propylene oxide 1301g, after equipressure obviously descends, add remaining propylene oxide again), pressure-controlling is at 0.0～0.4Mpa, add slaking, equipressure drops to reduce to and ends, cooling degassing discharging.
Embodiment 2:
In reactor, add the butylol polyether 500g that embodiment 1 makes, MMC catalyzer 0.075g, displacement N
2Heat up after three times, temperature to 100 ℃, dewatered 40 minutes, and be warmed up to 130 ℃ again and add propylene oxide 1001g (add 30g earlier, pressure is 0.2～0.9Mpa, after equipressure obviously descends, add remaining propylene oxide again), pressure-controlling adds slaking at 0.0～0.4Mpa, equipressure drops to reduce to and ends, cooling degassing discharging.
Embodiment 3:
In reactor, add the butylol polyether 100g that embodiment 1 makes, MMC catalyzer 0.075g, displacement N
2Heat up after three times, temperature to 100 ℃ was dewatered 40 minutes, was warmed up to 135 ℃ again, add propylene oxide 1401g and (add 30g earlier, pressure is 0.2～0.9Mpa, after equipressure obviously descends, adds remaining propylene oxide again), pressure-controlling is at 0.0～0.4Mpa, add slaking, equipressure drops to reduce to and ends, cooling degassing discharging.
Embodiment 4:
In reactor, add the butylol polyether 50g that embodiment 2 makes, MMC catalyzer 0.075g, displacement N
2Heat up after three times, temperature to 100 ℃ was dewatered 40 minutes, was warmed up to 140 ℃ again, add propylene oxide 1451g and (add 30g earlier, pressure is 0.3～0.9Mpa, after equipressure obviously descends, adds remaining propylene oxide again), pressure-controlling is at 0.0～0.4Mpa, add slaking, equipressure drops to reduce to and ends, cooling degassing discharging.
The prepared butylol polyether of the various embodiments described above after tested, specific targets are as follows:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Molecular weight | 550 | 1602 | 8095 | 16213 |
| Degree of unsaturation | 0.0008 | 0.003 | 0.007 | 0.02 |
Estimating of molecular weight gets according to recording the conversion of polyethers hydroxyl value: 56100/ actual measurement hydroxyl value; The detection method of hydroxyl value is carried out according to GB GB 12008.3.
Degree of unsaturation is iodine number/25.4; The detection method of iodine number is carried out according to GB GB/T 13892.
Claims (2)
1, a kind of synthetic method of butylol polyether, with butanols or lower molecular weight butylol polyether is initiator, the mixture of propylene oxide or propylene oxide and oxyethane or butylene oxide ring is a chain extension agent, it is characterized in that to contain Co, Zn, the multi-metal cyanide of Pb metal ion is a catalyzer, in temperature is to react under 90～160 ℃ the condition, makes butylol polyether; The add-on of described catalyzer is 0.002～0.015% of the butylol polyether the finished product weight percent that makes.
2, press the synthetic method of the described butylol polyether of claim 1, the molecular weight and the corresponding degree of unsaturation that it is characterized in that the described butylol polyether that makes are respectively: molecular weight is that 300～1000 o'clock degrees of unsaturation are 0.01～0.0005, molecular weight is that 1000～2000 o'clock degrees of unsaturation are 0.0015～0.0006, molecular weight is that 2000～5000 o'clock degrees of unsaturation are 0.02～0.0006, and molecular weight is that 5000～25000 o'clock degrees of unsaturation are 0.05～0.001.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610154860A CN100588671C (en) | 2006-11-28 | 2006-11-28 | Synthesizing process of butylol polyether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610154860A CN100588671C (en) | 2006-11-28 | 2006-11-28 | Synthesizing process of butylol polyether |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN100999577A CN100999577A (en) | 2007-07-18 |
| CN100588671C true CN100588671C (en) | 2010-02-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610154860A Active CN100588671C (en) | 2006-11-28 | 2006-11-28 | Synthesizing process of butylol polyether |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593190B (en) * | 2018-12-07 | 2021-04-13 | 浙江皇马科技股份有限公司 | Synthesis method of butanol polyether with low unsaturation degree, high molecular weight and high activity |
| CN110922579B (en) * | 2019-12-06 | 2021-12-03 | 浙江皇马科技股份有限公司 | Synthesis method of polyether for low-modulus sealant |
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| Publication number | Publication date |
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| CN100999577A (en) | 2007-07-18 |
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Effective date of registration: 20100602 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 |