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A kind of isopentenol random polyether and preparation method thereof

A technology of prenyl alcohol polyoxyethylene ether and prenyl alcohol, which is applied in the field of prenyl alcohol EO/PO random polyether and its preparation, can solve the problem of poor concrete fluidity, affecting application performance, and effective content reduce problems such as improving slump retention performance, high double bond protection rate, and narrow molecular weight distribution

Active Publication Date: 2020-01-10
ZHEJIANG HUANGMA NEW MATERIALS TECH CO LTD
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Problems solved by technology

However, since the polyether side chains of pure EO are easy to form hydrogen bonds, the fluidity of concrete becomes poor
Fang Chenwei and others tried to introduce propylene oxide blocks in the side chain, but the block polyether has excellent foaming and air-entraining properties, resulting in excessive air content in the concrete, which affects the workability of the mixture and the mechanical properties of the molded products. and durability
Moreover, the three-block structure of PEO-PPO-PEO, monomer synthesis and preparation take a long time and the process is cumbersome
[0004] In order to overcome the obvious shortcomings of the above macromonomer structure in engineering, there is a Chinese published patent No. CN105504261 A, the patent name is: random copolyether macromonomer, water reducer prepared therefrom, preparation method and application, Provide a preparation method through random copolymerization, adopt one-step synthesis to obtain EO / PO random copolyether macromonomer with smaller hydrodynamic radius, but slightly increased steric hindrance effect, but after synthesizing the water reducer, At the same time, it increases the steric hindrance between the cement molecules, slows down the hydration with cement, and deteriorates the workability, which affects the workability of the mixture.
[0005] Simultaneously, the existing synthetic technology about prenyl alcohol polyoxyethylene ether, the patent No. disclosed in China is CN101928392A, and the patent name is: a kind of synthetic method of prenyl alcohol polyoxyethylene ether, has introduced prenyl alcohol polyoxyethylene ether in Solid sodium methoxide, sodium methoxide methanol solution, potassium hydroxide solid or aqueous solution, sodium hydroxide or aqueous solution, sodium, sodium isoenolate or a mixture of more than one of them react with ethylene oxide to form iso Pentenol 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 will be retained. The efficiency is 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, which will lead to a decrease in effective content and a broadening of molecular weight distribution. The bond retention rate is reduced, thereby affecting its application performance; and for sodium and isoamyl sodium enolate, the preparation conditions and quality of the catalyst sodium prenate and the addition method of catalyst sodium and sodium prenate will still affect the isopentyl sodium. The quality of enol 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

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  • A kind of isopentenol random polyether and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0032]The preparation method of a kind of prenol EO / PO random polyether of the present embodiment comprises the following steps: 1) add 21.6 parts by weight of prenol to the reaction kettle, add 0.45 parts by weight of catalyst metal in 30 minutes Sodium, the reaction temperature is controlled at 20-30°C, and the reaction time is 0.5h; after the reaction, the product is put into 411 parts by weight of isopentenol, replaced by nitrogen, the temperature is raised to 90°C, and 1579.5 parts by weight of ethylene oxide is introduced , control the reaction temperature to be 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 prenyl alcohol polyoxyethylene ether oligomer with a molecular weight of 400; 2) add 90 wt. The molecular weight obtained in the step 1) is 400 prenol polyoxyethylene ether oligomers, 1.8 parts by weight of catalyst metal sodium are added within 30 minutes, the reaction tempera...

Embodiment 2

[0034] The preparation method of a kind of prenol EO / PO random polyether of the present embodiment comprises the following steps: 1) add 18.8 parts by weight of prenol to the reaction kettle, add 0.32 parts by weight of catalyst metal in 50 minutes Potassium, the reaction temperature is controlled at 25-35°C, and the reaction time is 0.5h; after the reaction, the product is put into 200.5 parts by weight of prenyl alcohol, replaced by nitrogen, the temperature is raised to 90°C, and 928.2 parts by weight of ethylene oxide is introduced , control the reaction temperature to be 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 prenyl alcohol polyoxyethylene ether oligomer with a molecular weight of 450; 2) add 84 wt. 2.4 parts by weight of catalyst metal potassium are added within 50 minutes to the prenol polyoxyethylene ether oligomer with a molecular weight of 450 obtained in the step 1) de...

Embodiment 3

[0036] The preparation method of a kind of prenol EO / PO random polyether of the present embodiment comprises the following steps: 1) add 17 parts by weight of prenol to the reaction kettle, add 0.21 parts by weight of sodium metal in 50 minutes and 0.21 parts by weight of potassium metal catalyst, the reaction temperature is controlled to be 30-40°C, and the reaction time is 0.8h; after the reaction, the product is put into 159.4 parts by weight of prenol, replaced with nitrogen, heated to 90°C, and introduced into 746.7 Parts by weight of ethylene oxide, the controlled reaction temperature is 90-105°C, and the reaction time is 5.5h; 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 450; 2) in The molecular weight that adds 84 parts by weight described step 1) in the reactor is the isopentenol polyoxyethylene ether oligomer of 450, adds 1.5 parts by weight sodium met...

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Abstract

The invention relates to an isopentenyl alcohol random polyether and a preparation method thereof, and belongs to the technical field of polyether compound synthesis in organic chemistry. According to the preparation method, at first, part of isopentenyl alcohol and a catalyst (A) carry out reactions, then the reaction system is added into residual isopentenyl alcohol, ethylene oxide is introduced into the mixture to carry out reactions to obtain oligomer; part of obtained oligomer and a catalyst (B) carry out reactions, then the reaction system is added into residual oligomer, and a mixture of ethylene oxide and propylene oxide is introduced into the mixture to carry out reactions to obtain isopentenyl alcohol random polyether. The isopentenyl alcohol random polyether is used to prepare a polycarboxylic acid water reducer, the quality of prepared isopentenyl alcohol EO / PO random polyether is stable, the application effect is good, and the isopentenyl alcohol random polyether is suitable for the synthesis of a high performance polycarboxylic acid water reducer.

Description

technical field [0001] The invention relates to a prenyl alcohol EO / PO random polyether (for convenience of description, hereinafter may also be abbreviated as prenyl alcohol random polyether) and a preparation method thereof, belonging to the synthesis technology of polyether compounds in organic chemistry field. Background technique [0002] Polycarboxylate superplasticizer is one of the most widely used cement and concrete admixtures in the construction industry. At present, mainly enol small molecular compounds are used as the initiator, and under the condition of alkali metal hydroxide as the catalyst, unsaturated polyether macromonomers with different molecular weights are reacted, and then reacted with small molecular units such as acrylic acid and maleic anhydride. The body is subjected to aqueous solution free radical polymerization to obtain a polycarboxylate water reducer. [0003] This type of water-reducing agent has a high water-reducing rate. Compared with n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08F283/06C08F220/06C04B24/26C04B103/30
CPCC04B24/2605C04B2103/0059C04B2103/302C08F283/065C08G65/2609C08G65/2648C08G2650/58C08F220/06
Inventor 董楠尹红金一丰万庆梅杜明强赵兴军
Owner ZHEJIANG HUANGMA NEW MATERIALS TECH CO LTD