CN101445432A - Synthetic method of nonyl phenol polyethenoxy ether - Google Patents
Synthetic method of nonyl phenol polyethenoxy ether Download PDFInfo
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- CN101445432A CN101445432A CNA2008101639854A CN200810163985A CN101445432A CN 101445432 A CN101445432 A CN 101445432A CN A2008101639854 A CNA2008101639854 A CN A2008101639854A CN 200810163985 A CN200810163985 A CN 200810163985A CN 101445432 A CN101445432 A CN 101445432A
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- Prior art keywords
- nonyl phenol
- polyethenoxy ether
- phenol polyethenoxy
- phenol poly
- oxypropylene ether
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Abstract
The invention relates to a synthetic method of nonyl phenol polyethenoxy ether, which belongs to the technical field of organic compound synthesizing. Taking nonyl phenol polyethenoxy ether low polymer as an initiator, propylene oxide as a chain extender and multi-metal cyanide (MMC) containing metallic ions such as Co, Zn, Pb, and the like as catalyst, the reaction is carried out at the temperature of 90 to 180 DEG C, so that the nonyl phenol polyethenoxy ether is obtained; and the amount of adding of the catalyst of multi-metal cyanide (MMC) accounts for 0.001 to 0.01 percent by weight of the obtained finished product of nonyl phenol polyethenoxy ether. The invention has simple process, no poisonous and harmful substance, high reactive behavior, short reaction period and reduction of the reaction time by at least a half; the molecular weight of the obtained has narrow distribution, the coefficient of distribution is smaller than 1.24 (the coefficient of distribution of the prior product is 1.2 to 1.8); and the degree of unsaturation of the obtained nonyl phenol polyethenoxy ether is obviously reduced (the degree of unsaturation of the prior product is larger than 0.08).
Description
Technical field
The present invention relates to a kind of synthetic method of nonyl phenol poly-oxypropylene ether, belong to technical field of organic compound synthesis.
Background technology
As everyone knows, do catalyst reaction with KOH, NaOH or sodium methylate, the nonyl phenol poly-oxypropylene ether unsaturated value that directly makes all very high (greater than 0.08), and also molecular weight is also done not quite (generally less than 2000), the product by product of making is many, can not production high viscosity high-molecular weight product.
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 nonyl phenol poly-oxypropylene ether of production cycle.
The present invention is the synthetic method of nonyl phenol poly-oxypropylene ether, it is characterized in that with the nonyl phenol poly-oxypropylene ether oligopolymer be initiator, propylene oxide is a chain extension agent, with the multi-metal cyanide (MMC) that contains metal ions such as Co, Zn, Pb is catalyzer, be to react under 90～180 ℃ the condition in temperature, make nonyl phenol poly-oxypropylene ether.
The add-on of described multi-metal cyanide catalyzer can be 0.001～0.01% of the nonyl phenol poly-oxypropylene ether the finished product weight percent that makes.
The molecular weight of described nonyl phenol poly-oxypropylene ether oligopolymer can be 200～1000.
Described nonyl phenol poly-oxypropylene ether oligopolymer can nonyl phenol be a raw material, KOH or NaOH or CH
3ONa is a catalyzer, and propylene oxide is a chain extension agent, in temperature is to react under 90～180 ℃ the condition to make.
It is initiator that the present invention adopts the nonyl phenol poly-oxypropylene ether oligopolymer, the multi-metal cyanide (MMC) that contains metal ions such as Co, Zn, Pb is a catalyzer, having solved in the prior art when the preparation nonyl phenol poly-oxypropylene ether molecular weight does not high, the degree of unsaturation height, the problem that postprocessing working procedures is numerous and diverse.Compared with prior art, have following outstanding advantage and positively effect:
1, technology is simple, and does not produce hazardous and noxious substances, the reactive behavior height, and reaction time is short, and the reaction times can shorten half at least.
2, the nonyl phenol poly-oxypropylene ether narrow molecular weight distribution of preparing, distribution coefficient is less than 1.24 (original product is 1.2～1.8); Degree of unsaturation obviously reduces (original all greater than 0.08).
3, the nonyl phenol poly-oxypropylene ether steady quality of preparing, reaction temperature and, the controllable-viscosity scope is big, controllability is good, lighter color, outward appearance is bright.
Molecular weight and corresponding unsaturated value by the nonyl phenol poly-oxypropylene ether of the method for the invention preparation are respectively: molecular weight 300～1000 unsaturated values are 0.001～0.01%, molecular weight 1000～2000 unsaturated values are 0.015～0.001%, molecular weight 2000～5000 unsaturated values are 0.002～0.02%, and molecular weight 5000～8000 unsaturated values are 0.002～0.03%.
Embodiment
The preparation of reactor before implementing: with distilled water the 2.5L autoclave is washed several times earlier, till clean, dried reactor, be cooled to after 30～60 ℃ of temperature standby.
Embodiment 1: add nonyl phenol 200g by prior art in reactor, KOH (solid) 1.9g, displacement N
2Heat up after three times, temperature to 100 ℃ adds propylene oxide 430g, adds equipressure and drops to reduce to and end the cooling degassing.Add the phosphoric acid neutralization, and the discharging of the polyethers sorbent material of 5～10% distilled water and 0.02～0.1% intensification dehydration after-filtration, make the nonyl phenol poly-oxypropylene ether oligopolymer.
Embodiment 2: add the nonyl phenol poly-oxypropylene ether oligopolymer 500g that embodiment 1 makes in reactor, MMC catalyzer 0.25g, displacement N
2Heat up after three times, 100 ℃, after the half an hour of dewatering,, temperature is transferred to 125 ℃ and is added propylene oxide 1001g.Add slaking, equipressure drops to reduce to and ends, cooling degassing discharging.
Embodiment 3: add the nonyl phenol poly-oxypropylene ether oligopolymer 100g that embodiment 1 makes in reactor, MMC catalyzer 0.032g, displacement N
2Heat up after three times, temperature to 100 ℃, after dehydration half an hour, temperature is transferred to 150 ℃ and is added propylene oxide 630.Add slaking, equipressure drops to reduce to and ends, cooling degassing discharging.
Embodiment 4: add the nonyl phenol poly-oxypropylene ether oligopolymer 100g that embodiment 1 makes in reactor, MMC catalyzer 0.04g, displacement N
2Heat up after three times, after temperature to 108 ℃ dehydration half an hour, temperature is transferred to 105 ℃ of mixture 1065g that add propylene oxide.Add slaking, equipressure drops to reduce to and ends, cooling degassing discharging.
Specific targets are as follows after tested for the prepared nonyl phenol poly-oxypropylene ether of the various embodiments described above:
| Embodiment | Molecular weight | Unsaturated value | Catalyst levels (%) |
| 1 | 690 | 0.0015 | 0.247(KOH) |
| 2 | 2065 | 0.002 | 0.006(MMC) |
| 3 | 5002 | 0.01 | 0.0033(MMC) |
| 4 | 7998 | 0.025 | 0.0026(MMC) |
Claims (4)
1, a kind of synthetic method of nonyl phenol poly-oxypropylene ether, it is characterized in that with the nonyl phenol poly-oxypropylene ether oligopolymer be initiator, propylene oxide is a chain extension agent, with the multi-metal cyanide (MMC) that contains metal ions such as Co, Zn, Pb is catalyzer, be to react under 90～180 ℃ the condition in temperature, make nonyl phenol poly-oxypropylene ether.
2, by the synthetic method of the described a kind of nonyl phenol poly-oxypropylene ether of claim 1, the add-on that it is characterized in that described multi-metal cyanide catalyzer is 0.001～0.01% of the nonyl phenol poly-oxypropylene ether the finished product weight percent that makes.
3, by the synthetic method of the described a kind of nonyl phenol poly-oxypropylene ether of claim 1, the molecular weight that it is characterized in that described nonyl phenol poly-oxypropylene ether oligopolymer is 200～1000.
4, by the synthetic method of claim 1 or 3 described a kind of nonyl phenol poly-oxypropylene ethers, it is characterized in that described nonyl phenol poly-oxypropylene ether oligopolymer is raw material with the nonyl phenol, KOH or NaOH or CH
3ONa is a catalyzer, and propylene oxide is a chain extension agent, in temperature is to react under 90～180 ℃ the condition to make.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101639854A CN101445432A (en) | 2008-12-30 | 2008-12-30 | Synthetic method of nonyl phenol polyethenoxy ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101639854A CN101445432A (en) | 2008-12-30 | 2008-12-30 | Synthetic method of nonyl phenol polyethenoxy ether |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101445432A true CN101445432A (en) | 2009-06-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101639854A Pending CN101445432A (en) | 2008-12-30 | 2008-12-30 | Synthetic method of nonyl phenol polyethenoxy ether |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021109557A1 (en) * | 2019-12-06 | 2021-06-10 | 浙江皇马科技股份有限公司 | Synthetic method for polyether for low modulus sealant |
-
2008
- 2008-12-30 CN CNA2008101639854A patent/CN101445432A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021109557A1 (en) * | 2019-12-06 | 2021-06-10 | 浙江皇马科技股份有限公司 | Synthetic method for polyether for low modulus sealant |
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Open date: 20090603 |