CN101260027A - Method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether - Google Patents
Method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether Download PDFInfo
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- CN101260027A CN101260027A CNA2008100548294A CN200810054829A CN101260027A CN 101260027 A CN101260027 A CN 101260027A CN A2008100548294 A CNA2008100548294 A CN A2008100548294A CN 200810054829 A CN200810054829 A CN 200810054829A CN 101260027 A CN101260027 A CN 101260027A
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- polyoxyethylene ether
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Abstract
The invention relates to a method for preparing narrow distribution fatty alcohol polyoxyethylene ether, comprising the following steps that: alcohol ether raw material is added to a feeder of a molecular distillation apparatus; under the conditions that: the evaporation temperature of a molecular distiller is 70-220 DEG C; a condenser is at the temperature of 0-30 DEG C and at the pressure of 0.1-300 Pa; the rotating speed of a film wiper is 0-1000 rpm, the alcohol ether raw material enters the molecular distillation apparatus from the feeder at the feeding speed of 0.01-100 Kg/h, so as to remove light components in the alcohol ether raw material and obtain primary distillation heavy components; the primary distillation heavy components are added into the feeder of the molecular distillation apparatus for carrying out secondary distillation and removing the heavy components in the primary distillation heavy components; the light components obtained in secondary distillation are just the narrow distribution fatty alcohol polyoxyethylene ether. The method has the advantages of simple process, short operation time, as well as high quality and yield coefficient of products.
Description
Technical field
The invention belongs to a kind of method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether, specifically a kind of physical method that adopts the molecular distillation method to prepare narrow distribution aliphatic alcohol polyoxyethylene ether.
Background technology
Fatty alcohol-polyoxyethylene ether is called for short alcohol ether (AEO
n), n represents average oxyethane (EO) adduction number, is the important nonionogenic tenside of a class, general formula is C
nH
2n+1-(OCH
2CH
2)
m-OH.Alcohol ether and derivative thereof have good decontamination, wetting and emulsification dispersive ability, little to skin irritation, biological degradability is good, the application conditions gentleness, and can obtain the product of different EO adduction numbers, thereby be widely used in daily chemical industry and other manufactures by the ratio that changes initiator and oxyethane.Its relative molecular weight distribution width be the principal element that influences the product physical and chemical performance [Duan Shiduo. nonionogenic tenside [M]. Beijing: China Railway Press, 1990.], studies show that [Xie Wenlei, Chen Yiqin. the narrow distribution ethoxylation of Fatty Alcohol(C12-C14 and C12-C18) technical progress [J]. the Zhengzhou Grain College journal, 1995,4:84～91.], compare with the wide molecular weight distribution ethoxylate, narrow distribution alcohol ether has many incomparable advantages: active principle content height, and smell is little; Pour point is low, good fluidity, save energy aspect transportation and storage; Smog is little in drying process with atomizing, reduces environmental pollution, improves operating condition; Better compatibility is arranged; Dirt there is better detergency; Advantage such as the derivative behavior of gained is superior when deriving (sulfonation, carboxymethylation).Therefore, how to obtain the alcohol ether of narrow molecular weight distributions, be the research topic that people paid close attention to for a long time always, the method for preparing at present narrow distribution aliphatic alcohol polyoxyethylene ether mainly realizes by ethoxylation catalyst, but the low [Cheng Lvbai of dispersion index of the alcohol ether of this method preparation, the narrow distribution technique of Fatty Alcohol(C12-C14 and C12-C18) ethoxylation [J]. daily chemical industry, 1991 (4): 21-27.], EO distributes widely, is unfavorable for the production and the application of product.
Summary of the invention
It is simple that the present invention provides a kind of technology, the product yield height, and the free of contamination employing molecular distillation of process method prepares the method for the high narrow distribution aliphatic alcohol polyoxyethylene ether of dispersion index.
The present invention is achieved in that and adopts molecular distillation apparatus to prepare narrow distribution aliphatic alcohol polyoxyethylene ether, it is characterized in that adopting following processing condition to operate:
(1) the raw material alcohol ether is added in the feeder of molecular distillation apparatus;
(2) vaporization temperature of setting molecular still is 70～220 ℃, and condenser temperature is 0～30 ℃, opens rotary-vane vaccum pump and oil diffusion pump, and making system operation pressure is 0.1～300Pa;
(3) begin charging when above-mentioned processing parameter reaches set(ting)value, feeding rate is 0.01～100Kg/h, and the blade applicator rotating speed is 1～1000rpm;
(4) the raw material alcohol ether removes the light component in the raw material alcohol ether in feeder enters molecular distillation apparatus, and light component becomes liquid through condenser condenses, obtains the single flash heavy component;
(5) the single flash heavy component is added in the feeder of molecular distillation apparatus, carry out second distillation, 130～250 ℃ of the vaporization temperatures of setting molecular still, 0～30 ℃ of condenser temperature, system operation pressure 0.1～300Pa begins charging when processing parameter reaches set(ting)value, feeding rate is 0.01～100Kg/h, the blade applicator rotating speed is 1～1000rpm, removes the light component that heavy component second distillation wherein obtains and is narrow distribution aliphatic alcohol polyoxyethylene ether.
The average EO adduction number of described feedstock fat polyoxyethylenated alcohol is 1～20, and alkyl carbon chain is that carbon number is 8～18 natural or synthetic side chain or straight-chain alkyl.
The present invention compares with the method for the narrow distribution ethoxylation catalyst of existing use catalysis synthesis of narrow distribution alcohol ether has following advantage:
Technology is simple, the operating time is short, service temperature is low, distill low, the separated material heated time weak point of pressure, product quality and product yield height.And, the main component of the light component that removes through single flash is low EO adduction array part, can be used as raw material once more with oxyethane generation ethoxylation, the synthetic alcohol ether that possesses desirable EO adduction number, the low EO adduction that also can be used as narrow distribution is counted the alcohol ether commodity and is directly used; The heavy component that removes through second distillation is that high EO adduction is counted alcohol ether, also can be directly as the alcohol ether commodity use of narrow distribution, and the each component in the raw material all is fully used.
Embodiment
Embodiment 1
The feedstock fat polyoxyethylenated alcohol AEO that in the feeder of molecular distillation apparatus, adds 100g
3(with 12 carbon and 14 carbon mixed fatty alcohols is raw material, gets through ethoxylation), this raw material A EO
3In free alkyl alcohol content be 20.9%, its dispersion index is 77.8%.The vaporization temperature of setting molecular still is 90 ℃, and condenser temperature is 10 ℃, opens rotary-vane vaccum pump and oil diffusion pump, making system operation pressure is 30Pa, can begin charging when processing parameter reaches set(ting)value, feeding rate is 60g/h, and the blade applicator rotating speed is 170rpm.The raw material alcohol ether under the effect of running up of knifing rotor, is evenly distributed on the hot face in feeder enters molecular distillation apparatus.Raw material is heated on hot face, under high vacuum condition, remove the light component (being mainly free alcohol) in the raw material alcohol ether, light component becomes liquid through condenser condenses, flow into light component receiving flask along prolong, heavy component flows into the heavy component receiving flask along the distiller inwall, is the single flash heavy component.After still-process finishes, get light component 28.3g, heavy component 71.7g; With the single flash heavy component as raw material, the vaporization temperature of setting molecular still is 150 ℃, condenser temperature is 10 ℃, system operation pressure is 40Pa, can begin charging when processing parameter reaches set(ting)value, feeding rate is 50g/h, and the blade applicator rotating speed is 200rpm, obtain light component 45.3g and be product, vinasse 26.4g.Free alkyl alcohol content in the product is reduced to 3.2%, and dispersion index is 96.8%.
The finished product of above embodiment are composed as follows:
Material mass percentage ratio/%
C
12OH 1.54
C
14OH 1.66
C
12EO
1 6.65
C
14EO
1 5.97
C
12EO
2 28.48
C
14EO
2 9.19
C
12EO
3 26.73
C
14EO
3 5.08
C
12EO
4 10.48
C
14EO
4 1.73
C
12EO
5 2.26
C
14EO
5 0.32
Embodiment 2
The feedstock fat polyoxyethylenated alcohol AEO that in the feeder of molecular distillation apparatus, adds 10Kg
3(with 12 carbon and 14 carbon mixed fatty alcohols is raw material, gets through ethoxylation), this raw material A EO
3In free alkyl alcohol content be 12.3%, its dispersion index is 87.1%.The vaporization temperature of setting molecular still is 120 ℃, and condenser temperature is 15 ℃, opens rotary-vane vaccum pump and oil diffusion pump, making system operation pressure is 50Pa, can begin charging when processing parameter reaches set(ting)value, feeding rate is 9Kg/h, and the blade applicator rotating speed is 500rpm.The raw material alcohol ether under the effect of running up of knifing rotor, is evenly distributed on the hot face in feeder enters molecular distillation apparatus.Raw material is heated on hot face, under high vacuum condition, remove the light component (being mainly free alcohol) in the raw material alcohol ether, light component becomes liquid through condenser condenses, flow into light component receiving flask along prolong, heavy component flows into the heavy component receiving flask along the distiller inwall, is the single flash heavy component.After still-process finishes, get light component 3.12Kg, heavy component 6.88Kg; With the single flash heavy component as raw material, the vaporization temperature of setting molecular still is 170 ℃, condenser temperature is 20 ℃, system operation pressure is 60Pa, begin charging when processing parameter reaches set(ting)value, feeding rate is 10Kg/h, and the blade applicator rotating speed is 400rpm, obtain light component 4.87Kg and be product, vinasse 2.01Kg.Free alkyl alcohol content in the product is reduced to 3.8%, and dispersion index is 96.2%.
The finished product of above embodiment are composed as follows:
Material mass percentage ratio/%
C
12OH 2.04
C
14OH 1.76
C
12EO
1 4.37
C
14EO
1 1.25
C
12EO
2 26.04
C
14EO
2 9.01
C
12EO
3 28.82
C
14EO
3 7.13
C
12EO
4 12.76
C
14EO
4 2.52
C
12EO
5 3.56
C
14EO
5 0.74
Embodiment 3
The feedstock fat polyoxyethylenated alcohol AEO that in the feeder of molecular distillation apparatus, adds 20Kg
3(with 12 carbon and 14 carbon mixed fatty alcohols is raw material, gets through ethoxylation), this raw material A EO
3In free alkyl alcohol content be 30.1%, its dispersion index is 69.7%.The vaporization temperature of setting molecular still is 140 ℃, and condenser temperature is 25 ℃, opens rotary-vane vaccum pump and oil diffusion pump, making system operation pressure is 100Pa, can begin charging when processing parameter reaches set(ting)value, feeding rate is 24Kg/h, and the blade applicator rotating speed is 240rpm.The raw material alcohol ether under the effect of running up of knifing rotor, is evenly distributed on the hot face in feeder enters molecular distillation apparatus.Raw material is heated on hot face, under high vacuum condition, remove the light component (being mainly free alcohol) in the raw material alcohol ether, light component becomes liquid through condenser condenses, flow into light component receiving flask along prolong, heavy component flows into the heavy component receiving flask along the distiller inwall, is the single flash heavy component.After still-process finishes, get light component 7.96Kg, heavy component 12.04Kg; With the single flash heavy component as raw material, the vaporization temperature of setting molecular still is 130 ℃, condenser temperature is 20 ℃, system operation pressure is 20Pa, begin charging when processing parameter reaches set(ting)value, feeding rate is 16Kg/h, and the blade applicator rotating speed is 320rpm, obtain light component 8.18Kg and be product, vinasse 3.86Kg.Free alkyl alcohol content in the product is reduced to 5.0%, and dispersion index is 95.0%.
The finished product of above embodiment are composed as follows:
Material mass percentage ratio/%
C
12OH 3.88
C
14OH 1.12
C
12EO
1 6.02
C
14EO
1 2.35
C
12EO
2 27.44
C
14EO
2 8.53
C
12EO
3 29.17
C
14EO
3 7.54
C
12EO
4 10.08
C
14EO
4 1.99
C
12EO
5 1.42
C
14EO
5 0.46。
Claims (3)
1, a kind of method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether is characterized in that comprising the steps:
(1) the raw material alcohol ether is added in the feeder of molecular distillation apparatus;
(2) vaporization temperature of setting molecular still is 70～220 ℃, and condenser temperature is 0～30 ℃, opens rotary-vane vaccum pump and oil diffusion pump, and making system operation pressure is 0.1～300Pa;
(3) begin charging when above-mentioned processing parameter reaches set(ting)value, feeding rate is 0.01～100Kg/h, and the blade applicator rotating speed is 1～1000rpm;
(4) the raw material alcohol ether removes the light component in the raw material alcohol ether in feeder enters molecular distillation apparatus, and light component becomes liquid through condenser condenses, obtains the single flash heavy component;
(5) the single flash heavy component is added in the feeder of molecular distillation apparatus, carry out second distillation, 130～250 ℃ of the vaporization temperatures of setting molecular still, 0～30 ℃ of condenser temperature, system operation pressure 0.1～300Pa begins charging when processing parameter reaches set(ting)value, feeding rate is 0.01～100Kg/h, the blade applicator rotating speed is 1～1000rpm, removes the light component that heavy component second distillation wherein obtains and is narrow distribution aliphatic alcohol polyoxyethylene ether.
2, a kind of method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether as claimed in claim 1 is characterized in that the average EO adduction number of described feedstock fat polyoxyethylenated alcohol is 1～20
3, a kind of method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether as claimed in claim 1, its feature is that carbon number is 8～18 natural or synthetic side chain or straight-chain alkyl at the alkyl carbon chain of described feedstock fat polyoxyethylenated alcohol.
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|---|---|---|---|
| CNA2008100548294A CN101260027A (en) | 2008-04-15 | 2008-04-15 | Method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether |
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|---|---|---|---|
| CNA2008100548294A CN101260027A (en) | 2008-04-15 | 2008-04-15 | Method for preparing narrow distribution aliphatic alcohol polyoxyethylene ether |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102477154A (en) * | 2012-02-28 | 2012-05-30 | 三江化工有限公司 | Preparation method of fatty alcohol polyoxyethylene ether |
| CN102634004A (en) * | 2012-03-15 | 2012-08-15 | 上海多纶化工有限公司 | Catalyst for synthesizing heterogeneous alcohol polyoxyethylene ether |
| CN102898327A (en) * | 2012-10-26 | 2013-01-30 | 山东师范大学 | Synthesis method for dimethyl azodicarboxylate and intermediate thereof |
| CN111040888A (en) * | 2020-01-17 | 2020-04-21 | 重庆理工大学 | Water-based cleaning agent with strong dispersing ability and cleaning method thereof |
| CN112354478A (en) * | 2020-11-02 | 2021-02-12 | 中国日用化学研究院有限公司 | Ultra-narrow distribution fatty alcohol ether and ultra-narrow distribution fatty alcohol ether sulfate compound system and continuous preparation method thereof |
-
2008
- 2008-04-15 CN CNA2008100548294A patent/CN101260027A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102477154A (en) * | 2012-02-28 | 2012-05-30 | 三江化工有限公司 | Preparation method of fatty alcohol polyoxyethylene ether |
| CN102634004A (en) * | 2012-03-15 | 2012-08-15 | 上海多纶化工有限公司 | Catalyst for synthesizing heterogeneous alcohol polyoxyethylene ether |
| CN102634004B (en) * | 2012-03-15 | 2015-01-14 | 上海多纶化工有限公司 | Catalyst for synthesizing heterogeneous alcohol polyoxyethylene ether |
| CN102898327A (en) * | 2012-10-26 | 2013-01-30 | 山东师范大学 | Synthesis method for dimethyl azodicarboxylate and intermediate thereof |
| CN111040888A (en) * | 2020-01-17 | 2020-04-21 | 重庆理工大学 | Water-based cleaning agent with strong dispersing ability and cleaning method thereof |
| CN112354478A (en) * | 2020-11-02 | 2021-02-12 | 中国日用化学研究院有限公司 | Ultra-narrow distribution fatty alcohol ether and ultra-narrow distribution fatty alcohol ether sulfate compound system and continuous preparation method thereof |
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Open date: 20080910 |