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A preparation method of hydrophobic nano calcium carbonate filled polyurethane pervaporation membrane

A technology of pervaporation membrane and nano calcium carbonate, applied in chemical instruments and methods, semi-permeable membrane separation, membrane technology and other directions, can solve the complex membrane preparation process, film formation, poor mechanical properties, poor selectivity, etc. problem, to achieve the effects of excellent mechanical strength, good hydrophobic surface, and simple preparation process

Active Publication Date: 2017-10-13
ZIBO HUATIAN RUBBER & PLASTICS SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although organosilicon polymers have good separation effect, their own film-forming properties and mechanical properties are poor. Although fluorine-containing polymers have good hydrophobicity due to fluorine atoms, their selectivity is not good and the cost is too high. Composite membranes The preparation process is relatively complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) Preparation of hydrophobic nano-calcium carbonate: Weigh 10g of dried nano-calcium carbonate, add 100g of deionized water, stir at 80°C to disperse evenly, then add 0.5g of oleic acid, stir at 80°C for 4h, filter, Finally, wash the nano-calcium carbonate repeatedly with the solvent n-hexane to remove excess oleic acid, dry it in a vacuum oven at 80°C, and obtain hydrophobic nano-calcium carbonate after grinding;

[0015] (2) Preparation of casting solution: Add xylene as a solvent in a reactor equipped with nitrogen protection, mechanical stirring and condensing reflux, and mix hydroxyl-terminated polybutadiene and toluene-2,4-diisocyanate into a mixture, Dissolve in xylene solvent, add catalyst dibutyltin dilaurate, stir evenly, react at 60°C for 3 hours, cool to room temperature, synthesize prepolymer, add hydrophobic nano-calcium carbonate, and add diphenylmethane drop by drop Diamine, heated up to 50° C. and stirred for 1 h to obtain a casting solution; the aver...

Embodiment 2

[0019] (1) Preparation of hydrophobic nano-calcium carbonate: Weigh 10g of dried nano-calcium carbonate, add 100g of deionized water, stir at 80°C to disperse evenly, then add 0.8g of stearic acid, stir at 80°C for 8h, filter , and then repeatedly wash the nano-calcium carbonate with solvent n-hexane to remove excess stearic acid, place it in a vacuum oven at 80°C for drying, and grind to obtain hydrophobic nano-calcium carbonate;

[0020] (2) Preparation of casting solution: Add xylene as a solvent in a reactor equipped with nitrogen protection, mechanical stirring and condensing reflux, and mix hydroxyl-terminated polybutadiene and toluene-2,4-diisocyanate into a mixture, Dissolve in xylene solvent, add catalyst dibutyltin dilaurate, stir evenly, react at 70°C for 1 hour, cool to room temperature, synthesize prepolymer, add hydrophobic nano-calcium carbonate, and add diphenylmethane drop by drop Diamine, heated up to 50° C. and stirred for 1 h to obtain a casting solution; t...

Embodiment 3

[0024] (1) Preparation of hydrophobic nano-calcium carbonate: Weigh 10g of dried nano-calcium carbonate, add 100g of deionized water, stir at 80°C to disperse evenly, then add 0.5g of oleic acid, stir at 80°C for 4h, filter, Finally, wash the nano-calcium carbonate repeatedly with the solvent n-hexane to remove excess oleic acid, dry it in a vacuum oven at 80°C, and obtain hydrophobic nano-calcium carbonate after grinding;

[0025](2) Preparation of casting solution: Add xylene as a solvent in a reactor equipped with nitrogen protection, mechanical stirring and condensing reflux, and mix hydroxyl-terminated polybutadiene and toluene-2,4-diisocyanate into a mixture, Dissolve in xylene solvent, add catalyst dibutyltin dilaurate, stir evenly, react at 70°C for 2 hours, cool to room temperature, synthesize prepolymer, add hydrophobic nano-calcium carbonate, and add diphenylmethane drop by drop Diamine, heated up to 50° C. and stirred for 1 h to obtain a casting solution; the avera...

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Abstract

The invention discloses a preparation method of a hydrophobic nano-grade calcium carbonate filled polyurethane pervaporation membrane. The method comprises the steps of: (1) dried nano-grade calcium carbonate is added into deionized water; a modifying agent is added, and a reaction is carried out while stirring; the material is repeatedly washed by using a solvent n-hexane, such that superfluous modifying agent is removed; the material is dried under vacuum and is ground, such that hydrophobic nano-grade calcium carbonate is obtained; (2) hydroxyl-terminated polybutadiene and toluene-2,4-diisocyanate are mixed and dissolved into a xylene solvent; a catalyst dibutyltin dilaurate is added; a prepolymer is obtained after a reaction; a proper amount of the hydrophobic nano-grade calcium carbonate is added, and diphenylmethane diamine is gradually dropped in; and a casting liquid is obtained after a reaction; and (3) the casting liquid is allowed to stand such that the casting liquid is de-aerated; the casting liquid is cast into a film on a polytetrafluoroethylene plate; the film is naturally air-dried under a normal temperature and is then vacuum dried, such that the pervaporation membrane is obtained. The method provided by the invention has the advantages of simple production steps, convenient operation, and low production cost. The film has good separation effect upon low-concentration butanol / water. The method and the film have good industrial application prospect.

Description

technical field [0001] The invention relates to a method for preparing a hydrophobic nano-calcium carbonate-filled polyurethane pervaporation membrane used for pervaporation preferentially permeating organic matter, and belongs to the technical field of pervaporation membrane separation. Background technique [0002] Affected by the energy crisis, oil prices have risen, butanol, as a new type of bioenergy, has received more and more attention. The product of butanol produced by biological fermentation (ABE fermentation) mainly contains acetone, butanol and ethanol, and the ratio of the three is 3:6:1. Mainly due to the inhibition of the product butanol, the total solvent concentration in the fermentation broth can only reach about 20gL -1 , lower production capacity. In order to solve the above problems, scientists try to couple some separation methods, such as pervaporation (PV), adsorption, liquid-liquid extraction, gas stripping and reverse osmosis, directly with the fe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L75/04C08K9/04C08K3/26C08G18/62B01D71/54B01D69/02B01D67/00
Inventor 娄尤来
Owner ZIBO HUATIAN RUBBER & PLASTICS SCI & TECH
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