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Method for determining alcohol hydroxyl value

A sample and weighing technology, applied in the field of analysis, can solve the problems of incomplete reaction, poor acylation ability, large operating error, etc., achieve high accuracy and reproducibility, accurate measurement results, and wide application range

Inactive Publication Date: 2014-09-03
LUZHOU NORTH CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the acylation ability of this method is relatively poor. During the reaction with the polymer polyether, the reaction is incomplete and the reaction sample is turbid, which increases the difficulty of judging the titration end point, making the determination of the phthalic anhydride acylation method The hydroxyl value is inaccurate, the error is large, and the error is even greater for different operators

Method used

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  • Method for determining alcohol hydroxyl value
  • Method for determining alcohol hydroxyl value
  • Method for determining alcohol hydroxyl value

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Embodiment 1 measures the hydroxyl value of PEG1000

[0074] Weigh 3.4571g of the PEG1000 sample and place it in a 500ml conical flask (do not allow the sample to contact the neck of the bottle), add 0.35g of anhydrous sodium acetate; draw 2mL of acetic anhydride with a pipette and add it to the conical flask containing the sample, Use a constant temperature heating magnetic stirrer to keep the system temperature at 85±2°C and continue heating for 5 to 10 minutes, add 25mL of distilled water, continue heating to boiling, and keep shaking to make the solution clear and transparent; remove the round bottom flask, cool to room temperature, add 0.5 mL phenolphthalein indicator (3-5 drops), neutralized with 0.5061mol / L sodium hydroxide standard solution until reddish, then accurately add 30mL of 0.5061mol / L sodium hydroxide solution (in order to prevent bumping, add a few glasses Beads), heated to boil for 10min, cooled rapidly to room temperature, added 0.5mL phenolphthalei...

Embodiment 2

[0076] Embodiment 2 measures the hydroxyl value of PEG2000

[0077] Weigh 3.3684g of the PEG2000 sample and place it in a 500ml conical flask (do not allow the sample to contact the neck of the bottle), add 0.35g of anhydrous sodium acetate; draw 2mL of acetic anhydride with a pipette and add it to the conical flask containing the sample, Use a constant temperature heating magnetic stirrer to keep the system temperature at 85±2°C and continue heating for 5 to 10 minutes, add 25ml of distilled water, continue heating to boiling, and keep shaking to make the solution clear and transparent. Take off the Erlenmeyer flask, cool to room temperature, add 0.5ml phenolphthalein indicator (3-5 drops), neutralize with 0.5061mol / L sodium hydroxide standard solution to reddish, then accurately add 30ml of 0.5061mol / L hydroxide Sodium solution (a few glass beads can be added to prevent bumping), heat to boil for 10 minutes, rapidly cool to room temperature, add 0.5ml phenolphthalein indicat...

Embodiment 3

[0079] Embodiment 3 measures the hydroxyl value of GAP

[0080] Weigh 3.4631g of the GAP sample and place it in a 500ml Erlenmeyer flask (do not allow the sample to come into contact with the neck of the bottle), add 0.35g of anhydrous sodium acetate; draw 2mL of acetic anhydride with a pipette and add it to the Erlenmeyer flask containing the sample, Use a constant temperature heating magnetic stirrer to keep the system temperature at 85±2°C and continue heating for 5 to 10 minutes, add 25ml of distilled water, continue heating to boiling, and keep shaking to make the solution clear and transparent. Take off the Erlenmeyer flask, cool to room temperature, add 0.5ml phenolphthalein indicator (3-5 drops), neutralize with 0.5061mol / L sodium hydroxide standard solution to reddish, then accurately add 30ml of 0.5061mol / L hydroxide Sodium solution (a few glass beads can be added to prevent bumping), heat to boil for 10 minutes, rapidly cool to room temperature, add 0.5ml phenolphth...

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Abstract

The invention belongs to the technical field of analysis, and specifically relates to a method for determining a polyether polyol hydroxyl value. The method comprises the steps of enabling alcohol and acetic anhydride to generate an esterification reaction by utilizing sodium acetate as a catalyst to generate ester and acetic acid, adding water to excess acetic anhydride to hydrolyze to generate acetic acid, neutralizing the acetic acid by utilizing aqueous alkali, adding excess aqueous alkali to cause the ester to generate a saponification reaction; after the saponification reaction is finished, titrating the residual alkali by utilizing acid solution; carrying out a blank test under the same conditions, and computing the content of hydroxyl in alcohol, wherein a difference of acid solutions consumed by the blank test and a sample is the amount of the alkali consumed by the saponification reaction of the ester. The method for determining the alcohol hydroxyl value can be applied to determining the amount of the hydroxyl value in the alcohol, and the accuracy and reproducibility are higher.

Description

technical field [0001] The invention belongs to the technical field of analysis, in particular to a method for measuring the hydroxyl value of polyether polyols. Background technique [0002] It is the current development trend of solid rocket propellants to replace traditional inert binders with energetic binders. Azide energetic prepolymers are a class of energetic polymers that have been studied more at present, among which azidoglycidyl ether (GAP), 3-azidomethyl-3-methylepoxybutylene (AMMO) and 3,3-bisazidomethyloxetane (BAMO) has a good application prospect. Accurately analyzing the properties of high-molecular-weight azide adhesives such as GAP, AMMO, and BAMO has become the key to the application of such products, especially the determination of the hydroxyl value, which directly affects the entire formulation system (curing agent, other Determination of binder and chain extender content) performance. [0003] The hydroxyl value refers to the number of milligrams ...

Claims

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Application Information

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IPC IPC(8): G01N31/20
Inventor 董军谷强毛长勇汤家全侯毅李彬刘金瑞王文彬孙建友
Owner LUZHOU NORTH CHEM IND
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