Method for preparing ester terminated allyl alcohol polyether

An allyl alcohol polyether and ester-based sealing technology is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of cumbersome steps, poor product molecular weight adjustability, and waste of raw materials The effect of simple process

Active Publication Date: 2010-05-05
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This traditional method, step is more loaded down with trivial details; Product molecular weight adjustability is relatively poor; Used carboxylic acid or carboxylic acid anhydride all must be excessive, could guarantee conversion rate, unreacted raw material (carboxylic acid or carboxylic anhydride) must be removed after reaction Removal, resulting in waste of raw materials; the reaction will also generate a large number of by-products, which require further continuous post-processing to continue to use

Method used

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  • Method for preparing ester terminated allyl alcohol polyether
  • Method for preparing ester terminated allyl alcohol polyether
  • Method for preparing ester terminated allyl alcohol polyether

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0028] Preparation of catalyst:

[0029] [Catalyst 1]

[0030] 49.2g Mg(NO 3 ) 2 ·6H 2 O, 26.6g Al 2 (SO 4 ) 3 ·18H 2 O, 7.1g CaCl 2 ·6H 2 O and 5.7g (CH 3 COO) 2 Ca·H 2 O was dissolved in 200g of deionized water to prepare a uniform mixed solution, and 200g was dissolved in 17.5g of NaOH and 43.3g of Na under strong stirring at 60℃ 2 CO 3 The deionized water solution was added dropwise to the above mixed solution. After 1 hour of dripping, the temperature was kept for 30 minutes, and then the reaction solution was allowed to stand at 65°C for 24 hours, filtered with suction, washed with distilled water to neutrality, and dried at 80°C under vacuum. It was calcined at 500°C for 5 hours, and after grinding, catalyst 1 was obtained.

[0031] [Catalyst 2]

[0032] 44.7g MgCl 2 ·6H 2 O, 54.1g MgSO 4 ·7H 2 O, 15.2g Al(NO 3 ) 3 ·9H 2 O, 9.6g AlCl 3 ·6H 2 O and 5.7g Ca(NO 3 ) 2 ·4H 2 O is dissolved in 300g of deionized water to prepare a uniform mixed solution, and 18.7g of NH is dissolved i...

Embodiment 1

[0037] Synthesis of acetyl ester group-terminated allyl alcohol polyether monomer: In a 1 liter dry stainless steel autoclave, add 10 g of anhydrous magnesium sulfate to dry for 48 hours 100 g of allyl acetate, 3.3 g of the above catalyst 1, and stir Mix well and seal the reactor. After evacuating the reaction kettle, replace the air in the kettle with nitrogen three times, heating to 100°C, while continuously introducing 440g of ethylene oxide, keeping the temperature at 100°C, and under the pressure of 0.2MPa, reacting until the pressure no longer drops, and then evacuating After maintaining the temperature to -0.08MPa and maintaining for 30 minutes, the temperature is lowered to 40°C, the material is discharged, and the solid catalyst is removed by filtration while hot to obtain an acetyl ester group-terminated polyoxyethylene ether monomer with an average molecular weight of 540.

Embodiment 2

[0039] Synthesis of propionyl ester group-terminated allyl alcohol polyether monomer: In a 1 liter dry stainless steel autoclave, add 11.2g molecular sieve drying treatment for 24 hours, 57g allyl propionate, 23.8g the above catalyst 2, and stir Mix well and seal the reactor. After the reactor was evacuated, the air in the reactor was replaced with nitrogen three times, and the temperature was raised to 120°C. At the same time, a mixture of 352g ethylene oxide and 112g propylene oxide was continuously introduced. The temperature was maintained at 120°C and the pressure was 0.5MPa. No more drop, then vacuumize to -0.08MPa, maintain for 30min, cool to 60℃, discharge, filter while hot to remove the solid catalyst, and obtain propionyl ester group-terminated allyl alcohol polyoxyethylene / polyoxyethylene with an average molecular weight of 1042 Polyoxypropylene random polyether monomer.

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Abstract

The invention provides a method for preparing ester terminated allyl alcohol polyether, which has simple process and realizes diversity of ester terminated allyl alcohol polyether monomer structure. The method for preparing the ester terminated allyl alcohol polyether comprises the following steps: allyl alkyl acid ester is used as initiator and ternary metal oxide is used as catalyst to ensure that oxirane and/or propylene epoxide perform a ring-opening polymerization reaction at 100-140 DEG C under the pressure of 0.1 to 0.6MPa; the ester terminated allyl alcohol polyether can be obtained after the catalyst is filtered and removed, wherein the ternary metal oxide catalyst is prepared from soluble salt of Mg, Al and Ca through alkaline precipitation and calcination. The preparation process is simple without using organic solvent, can be completed in one step by continuously adding materials in the same reactor. The prepared ester terminated allyl alcohol polyether monomer molecule has diverse structures, adjustable amphipathic property and controllable molecular weight, and can be polymerized with multiple unsaturated monomers.

Description

Technical field [0001] The invention relates to a method for preparing an ester group-terminated allyl alcohol polyether, belonging to the technical field of the synthesis of reactive end-terminated polyethers. Background technique [0002] The ester group-terminated allyl alcohol polyether means that the hydroxyl group at the end of the allyl alcohol polyether is replaced by an alkyl ester. Ester group-terminated allyl alcohol polyether monomers can be free radicals with other vinyl monomers (such as acrylic acid, acrylamide, styrene, vinyl acetate, sodium styrene sulfonate, itaconic acid, maleic anhydride, etc.) Copolymerization and reaction to form copolymers with different structures and different molecular weights. These copolymers are widely used as dispersants, concrete water reducers, adhesives, emulsifiers, scale inhibitors, antistatic agents, silicone modifiers, etc. . [0003] Generally, the synthesis of this ester group-terminated allyl alcohol polyether monomer is ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/26C07C67/00C07C69/16C07C69/28C07C69/025
Inventor 刘加平杨勇缪昌文冉千平张志勇周栋梁毛永琳
Owner JIANGSU SOBUTE NEW MATERIALS
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