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Preparation method for high unsaturated isoamyl alcohol polyoxyethylene ether

A technology of prenol polyoxyethylene ether and prenol, which is applied in the field of polyether synthesis in organic chemistry, can solve the problem that the molecular weight of polycarboxylic acid-based water reducing agent is difficult to meet the design requirements, the product has high PEG content, and The problems such as low flash point of pentenol can save the dehydration time, narrow molecular weight distribution and high relative molecular weight.

Active Publication Date: 2013-09-04
浙江三江化工新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis process of prenyl alcohol polyoxyethylene ether is relatively complicated, and there are few reports in literature and patents. Chinese published patent CN 101928392A records that sodium hydroxide, potassium hydroxide, sodium methylate and sodium, and sodium prenyl alcohol are used in traditional alkali catalysts. In the presence of prenyl alcohol, ethylene oxide is passed into the prenyl alcohol for condensation to prepare prenyl alcohol polyoxyethylene ether
This method has the following defects: the production process is complex and dangerous (the reaction time for preparing sodium prenolate from metal sodium and prenol is long, the flash point of prenol is low, and the reaction with metal sodium is prone to combustion), and the product PEG High content (low flash point of prenol, catalyst sodium hydroxide, potassium hydroxide, sodium methoxide and prenol can not remove water or methanol), low degree of unsaturation
The degree of unsaturation reflects the density of double bonds, and the lower degree of unsaturation will make the conversion rate of isopentenol polyoxyethylene ether further copolymerized with unsaturated compounds low, thereby affecting the grafting rate and reducing the polycarboxylic acid system. The molecular weight of the water agent is difficult to meet the design requirements

Method used

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  • Preparation method for high unsaturated isoamyl alcohol polyoxyethylene ether
  • Preparation method for high unsaturated isoamyl alcohol polyoxyethylene ether

Examples

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Embodiment 1

[0038] Example 1 Preparation of magnesium-aluminum inorganic composite catalyst 1

[0039] Mix and grind 0.01mol aluminum nitrate and 0.09mol magnesium nitrate, add 1000ml deionized water to fully disperse, add 0.1mol sodium hydroxide and 0.03mol sodium carbonate under stirring, raise the temperature to 70°C and continue stirring for 24 hours, then place in a 70°C water bath Stand and age for 24 hours, wash with suction and water, extrude the filter cake, dry at room temperature for 8 hours, then dry in an oven above 120°C until no weight loss, and grind for later use.

Embodiment 2

[0040] Example 2 Preparation of magnesium-aluminum inorganic composite catalyst 2

[0041] Mix and grind 0.01mol aluminum nitrate, 0.01mol aluminum sulfate, 0.01mol aluminum chloride, 0.1mol magnesium nitrate, 0.05mol magnesium chloride and 0.03mol ferric chloride, add 1000ml deionized water to fully disperse, add 0.2mol sodium hydroxide under stirring and 0.03mol sodium carbonate, heated up to 60°C and continued to stir for 24 hours, then stood and aged in a 70°C water bath for 24 hours, filtered and washed with water, extruded the filter cake, dried at room temperature for 8 hours, and then Dry in an oven at 120°C until there is no weight loss, and grind for later use.

Embodiment 3

[0042] Example 3 Preparation of magnesium-aluminum inorganic composite catalyst 3

[0043]Mix and grind 0.01mol aluminum sulfate, 0.19mol aluminum chloride, 0.04mol magnesium sulfate, 0.06mol magnesium nitrate, 0.1mol magnesium chloride, 0.04mol nickel chloride and 0.06mol iron oxide, add 1000ml deionized water to fully disperse, add under stirring 0.15mol sodium hydroxide and 0.03mol sodium carbonate, heated to 75°C and continued to stir for 24 hours, then left to age in a 70°C water bath for 24 hours, filtered and washed with water, extruded the filter cake, and dried at room temperature for 8 hours , and then dried in an oven above 120°C until no weight loss, and then ground for later use.

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Abstract

The invention relates to a preparation method for high unsaturated isoamyl alcohol polyoxyethylene ether, belongs to the technical filed of polyether synthesis in organic chemistry. The preparation method comprises the following process steps of 1) carrying out a condensation reaction by adding ethylene oxide in presence of a solid alkali catalyst of a magnesium-aluminum inorganic compound, with isoamyl alcohol as an initiator, so as to obtain an isoamyl alcohol oligomer; and 2) adding ethylene oxide in the isoamyl alcohol oligomer obtained by the step 1) again to carry out the condensation reaction, so as to obtain isoamyl alcohol polyoxyethylene ether. The preparation method is simple in process and safe; and the obtained isoamyl alcohol polyoxyethylene ether has narrow molecular weight distribution, relatively high molecular weight, few by-products and high degree of unsaturation.

Description

technical field [0001] The invention belongs to the technical field of polyether synthesis in organic chemistry, and in particular relates to a preparation method of prenol polyoxyethylene ether with high degree of unsaturation. Background technique [0002] Polycarboxylate high-performance water reducer is the third generation of high-performance water reducer developed after the common water reducer represented by wood calcium and the high-efficiency water reducer represented by naphthalene series. It is currently the most cutting-edge water reducer in the world. , A high-efficiency water reducer with the highest scientific and technological content, the best application prospects, and the best comprehensive performance. It has a high proportion of active ingredients and a concentrated molecular weight range. Compared with other water reducers, polycarboxylate water reducers not only have higher water reducing rate, but also keep slump for a long time, and the dosage is ve...

Claims

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Application Information

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IPC IPC(8): C08G65/28C04B24/32C04B103/30
Inventor 彭义秋
Owner 浙江三江化工新材料有限公司
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