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Preparation method of alkyl blocked allyl polyether

A technology of allyl-terminated polyether and alkyl polyether, which is applied in the field of preparation of alkyl-terminated allyl polyether, can solve the problems of troublesome post-processing, many side reactions, and increased side reactions, and achieve post-processing Convenient and simple, simplified reaction conditions, mild reaction conditions

Active Publication Date: 2011-03-02
GUANGDONG BIOMAX SIANDF NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if allyl polyether is used as an intermediate product, if it is directly produced by the downstream industry and used in the next step of synthesis, this method is relatively cumbersome, and this method has certain requirements for the pressure of the reaction.
Chinese patent CN 101543747A (disclosure date on September 30, 2009) provides a method for preparing allyl alkylphenol polyoxyethylene ether in a solvent medium. The method uses a solvent, and its disadvantage is that post-treatment is cumbersome, and Using alcohols as a solvent has many side reactions and reduces the yield. This method is not conducive to industrial production
Chinese patent CN 101628976A (disclosure date January 20, 2010) provides a method for preparing butyl-terminated allyl polyoxyethylene ether, using allyl polyoxyethylene ether and bromobutane as raw materials, and selecting two Step method, which requires high pressure for the reaction and relatively high cost
[0004] Chinese patents CN1563146, CN1311264 and other patents disclose the use of allyl alcohol polyether, alkaline slow-release microcapsules and dimethyl sulfate / diethyl sulfate one-step method to cap the polyether alkyl group. Moisture is generated during the process, which leads to an increase in side reactions during the etherification capping reaction, resulting in an increase in the amount of capping agent and troublesome product refining, which increases the cost of production
[0005] At present, there is a lack of a method for the preparation of alkyl-terminated allyl polyethers that are suitable for direct production in downstream industries and have low production costs.

Method used

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  • Preparation method of alkyl blocked allyl polyether
  • Preparation method of alkyl blocked allyl polyether
  • Preparation method of alkyl blocked allyl polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a four-necked flask equipped with a stirring device, a reflux condenser, a thermometer and a dropping funnel, add R to C 12 Fatty alcohol polyoxyethylene ether (I) (number of oxyethylene n=7) 247g, NaOH 21g, stirred and heated to 40°C, within 1.5 hours, 57g of allyl chloride was added dropwise, and then reacted at 100°C for 5 hours, After the reaction is completed, use 2g of glacial acetic acid to neutralize to neutral, distill under reduced pressure at 100-110°C for 1.5 hours, remove low boilers until the allyl chloride is basically removed, filter and separate the organic matter and the generated salt to obtain the target compound 240g, the yield is 90%, light yellow transparent liquid.

[0038] Spectral analysis of target compounds:

[0039] IR (KBr cm -1 ): 2917(C-H), 1645(C=C), through the division of characteristic absorption peaks, it is proved that the product structure contains carbon-carbon unsaturated double bond C=C, which shows that the main product ob...

Embodiment 2

[0042] In a four-necked flask equipped with a stirring device, a reflux condenser, a thermometer and a dropping funnel, add R to C 12 Isomerized alkyl alcohol polyoxyethylene ether (I) (oxyethylene number n=9) 188g, KOH 18g, stirred and heated to about 30°C, within 0.5 hours, 25g of allyl chloride was added dropwise, and then at 70°C React under low temperature for 6 hours. After the reaction is completed, use 10g of 35% hydrochloric acid solution to neutralize to neutrality. Distill under reduced pressure at 100-110°C for 1 hour, remove low boiling matter until allyl chloride is basically removed, and filter to separate organic matter. and the generated salt to obtain 165 g of the target compound, with a yield of 83%, and a yellow transparent liquid.

[0043] Spectral analysis of target compounds:

[0044] IR (KBr cm -1 ): 2924(C-H), 1647(C=C), through the division of characteristic absorption peaks, it is proved that the product structure contains carbon-carbon unsaturated...

Embodiment 3

[0047] In a three-neck flask equipped with a stirring device, a reflux condenser, a thermometer and a dropping funnel, add R to C 18Fatty alcohol polyoxyethylene ether (I) (oxyethylene number n=3) 502g, NaOH 60g, stirred and heated up to 50°C, within 3.0 hours, 143g of allyl chloride was added dropwise, and then reacted at 90°C for 3.5 hours, After the reaction is completed, use 7.5g of glacial acetic acid to neutralize to neutral, distill under reduced pressure at 100-110°C for 1.5 hours, remove low boilers until allyl chloride is basically removed, filter and separate organic matter and generated salts to obtain the target Compound 463g, yield 93%, light yellow transparent liquid.

[0048] Spectral analysis of target compounds:

[0049] IR (KBr cm -1 ): 2923(C-H), 1647(C=C), through the division of characteristic absorption peaks, it is proved that the product structure contains carbon-carbon unsaturated double bond C=C, which shows that the main product obtained is exactl...

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Abstract

The invention discloses a preparation method of alkyl blocked allyl polyether. The preparation method comprises the following steps: carrying out reaction on alkyl polyether and halogenated propylene under the action of alkali metal hydroxides without solvent to generate the alkyl blocked allyl polyether. The reaction of the preparation method is carried out under ordinary pressure, the reaction temperature is lower than 120 DEG C, and the preparation method has the advantages of high reaction yield and little pollution, and is suitable for production in downstream industry and directly used for next reaction. Compared with the traditional technology, the preparation method simplifies the reaction conditions and saves the cost. The prepared alkyl blocked allyl polyether is suitable for preparing blocked non-ionic surfactant with low surface tension, favorable emulsifying property and favorable nucleation property.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a preparation method of an alkyl-terminated allyl polyether. Background technique [0002] Allyl polyether has good hydrophilicity and superior emulsifying ability. It is a kind of nonionic surfactant with excellent performance. Because its end group has double bonds, it plays an important role in polymer synthesis. [0003] Chinese patent CN 101099926A (disclosure date on January 9, 2008) provides a method for preparing an alkyl-terminated allyl polyether, which uses allyl alcohol, ethylene oxide and propylene oxide as raw materials. In the presence of metal catalysts such as zinc hexaoxide cobaltate compounds, the terminal allyl polyether is prepared under conditions such as pressure ≤ 0.2 MPa, and then the hydroxyl group at the other end is replaced with an alkoxy group to obtain a terminal modified polyether. However, if allyl polyether is used as an intermedia...

Claims

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Application Information

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IPC IPC(8): C08G65/00C07C43/15C07C43/205C07C41/16
Inventor 黄振宏钟增培谢秀鸿
Owner GUANGDONG BIOMAX SIANDF NEW MATERIAL CO LTD
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