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Preparation method of isopentenol polyoxyethylene ether

A technology of prenol polyoxyethylene ether and isopentenol, which is applied in the field of preparation of prenol polyoxyethylene ether, can solve the problem of reducing the application effect of prenol polyoxyethylene ether and the retention rate of double bonds problems such as reduction and broadening of molecular weight distribution, to achieve the effect of high double bond retention rate, narrow molecular weight distribution and high effective content

Inactive Publication Date: 2013-12-25
ZHEJIANG LYUKEAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing synthesis technology about prenyl alcohol polyoxyethylene ether, China's published patent number is CN101928392A, patent name is: a kind of synthetic method of prenyl alcohol polyoxyethylene ether, introduces prenyl alcohol polyoxyethylene ether in solid methanol Sodium, sodium methoxide methanol solution, potassium hydroxide solid or aqueous solution, sodium hydroxide or aqueous solution, sodium, sodium isoenolate or a mixture of one or more of them react with ethylene oxide to form isopentene Alcohol polyoxyethylene ether, but for solid sodium methoxide and sodium methoxide methanol solution, more by-products such as polyethylene glycol monomethyl ether, etc. will be produced, and the effective content will be reduced, the molecular weight distribution will be broadened, and the double bond retention rate will be reduced. , thereby affecting its application performance; and for potassium hydroxide solid or aqueous solution, sodium hydroxide solid or aqueous solution, more by-products such as polyethylene glycol will be produced, and at the same time, it will lead to a decrease in effective content, a broadening of molecular weight distribution, and double bond retention rate decreases, thereby affecting its application performance; and for sodium and iso-sodium enolate, the preparation conditions and quality of the catalyst sodium prenolate and the addition method of catalyst sodium and sodium prenolate will still affect the prenolate. The quality of polyoxyethylene ether leads to the generation of by-products such as polyethylene glycol, the broadening of molecular weight distribution, and the reduction of double bond retention, thereby reducing the application effect of isopentenol polyoxyethylene ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation method of prenyl alcohol polyoxyethylene ether in this embodiment comprises the following steps: 1) Add 21.6 parts by weight of prenyl alcohol into the reaction kettle, add 0.45 parts by weight of catalyst metal sodium within 30 minutes, and control The reaction temperature is 20~30°C, and the reaction time is 0.5h; after the reaction, put the product into 411 parts by weight of prenyl alcohol, replace it with nitrogen, raise the temperature to 90°C, and feed 1076.5 parts by weight of ethylene oxide to control the reaction The temperature is 90~105°C, and the reaction time is 4.0h; after the reaction, the temperature is lowered to 70°C and the material is discharged to obtain a prenol polyoxyethylene ether oligomer with a molecular weight of 300; 2) Add 90 parts by weight of the Step 1) The obtained isopentenol polyoxyethylene ether oligomer with a molecular weight of 300, add 1.8 parts by weight of catalyst metal sodium within 30 minutes, control the react...

Embodiment 2

[0026]The preparation method of a kind of prenol polyoxyethylene ether of this embodiment comprises the following steps: 1) Add 18.8 parts by weight of prenol into the reaction kettle, add 0.32 parts by weight of catalyst metal potassium within 50 minutes, control The reaction temperature is 25~35°C, and the reaction time is 0.5h; after the reaction, put the product into 200.5 parts by weight of prenyl alcohol, replace with nitrogen, raise the temperature to 90°C, and feed 673.2 parts by weight of ethylene oxide to control the reaction The temperature is 90~105°C, and the reaction time is 5.0h; after the reaction, the temperature is lowered to 70°C and the material is discharged to obtain a prenol polyoxyethylene ether oligomer with a molecular weight of 350; 2) Add 84 parts by weight of the Step 1) for the prenol polyoxyethylene ether oligomer with a molecular weight of 350, add 2.4 parts by weight of catalyst metal potassium within 50 minutes, control the reaction temperature...

Embodiment 3

[0033] A preparation method of prenyl alcohol polyoxyethylene ether in this embodiment includes the following steps: 1) Add 17 parts by weight of prenyl alcohol into the reaction kettle, add 0.21 parts by weight of sodium metal and 0.21 parts by weight of sodium metal in 50 minutes Part metal potassium catalyst, control the reaction temperature at 30~40°C, and the reaction time is 0.8h; after the reaction, put the product into 159.4 parts by weight of prenyl alcohol, replace with nitrogen, raise the temperature to 90°C, and pass 541.5 parts by weight of ring Ethylene oxide, the reaction temperature is controlled at 90~105°C, and the reaction time is 5.5h; after the reaction is completed, the temperature is lowered to 70°C and the material is discharged to obtain a prenol polyoxyethylene ether oligomer with a molecular weight of 350; 2) in the reaction kettle Add 84 parts by weight of the isopentenol polyoxyethylene ether oligomer with a molecular weight of 350 obtained in the s...

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Abstract

The invention discloses a preparation method of isopentenol polyoxyethylene ether. The method comprises the steps of: 1) firstly reacting 5-20wt% of prescribed dosage isopentenol with a catalyst, then putting the product into the remaining prescribed dosage isoprene, and introducing ethylene oxide to react so as to obtain an isopentenol polyoxyethylene ether oligomer with a molecular weight of 300-500; 2) reacting the prepared 5-20wt% of prescribed dosage isopentenol polyoxyethylene ether oligomer with the catalyst, then putting the product into the remaining prescribed dosage isopentenol polyoxyethylene ether oligomer, and introducing ethylene oxide to react so as to obtain isopentenol polyoxyethylene ether with a molecular weight of 500-5000. The product prepared by the invention has the advantages of low content of polyethylene glycol and other by-products, narrow molecular weight distribution, and high double bond protection rate, and is suitable for synthesis of polycarboxylate type high performance water reducing agents.

Description

technical field [0001] The invention relates to a preparation method of prenol polyoxyethylene ether, which belongs to the technical field of synthesis of polyether compounds in organic chemistry. Background technique [0002] Polycarboxylate water reducer has the advantages of high water reducing rate, small slump loss over time, low dosage, low concrete shrinkage, strong controllable molecular structure and environmental friendliness, which can greatly improve the working performance of concrete , greatly improve the compressive strength and durability of concrete, and are widely used in the field of concrete engineering construction such as railways and bridges. There are two ways to synthesize polycarboxylic acid-based water reducers. One is polyether without unsaturated double bonds, such as polyethylene glycol monomethyl ether MPEG. Acrylic acid is reacted to produce methacrylate or acrylate of polyethylene glycol monomethyl ether, and then it is copolymerized with mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C04B24/32
Inventor 王胜利金一丰董楠马定连万庆梅
Owner ZHEJIANG LYUKEAN CHEM
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