CN104020251A - Method for determining alcohol hydroxyl value - Google Patents
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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
The invention belongs to analysis technical field, be specifically related to a kind of method of measuring polyether glycol hydroxyl value.
Background technology
To replace the trend that traditional inert binder is current solid rocket propellant development containing energy bonding agent.It can prepolymer be that the more class of research is at present containing energy polymkeric substance that nitrine class contains, wherein the two azido-methyl oxa-fourth rings (BAMO) of nitrine glycidol ether (GAP), 3-azido-methyl-3-methyl epoxy butane (AMMO) and 3,3-have good application prospect.The performance of the nitrine family macromolecule amount bonding agents such as accurate analysis GAP, AMMO, BAMO becomes the key of this series products application, especially the mensuration of hydroxyl value, the performance of whole formula system while directly having affected adhesive application (determining of hardening agent, other cementing agent and chain extender content).
Hydroxyl value refers to milligram number, the i.e. mgKOH/g of the potassium hydroxide that the hydroxyl in 1g sample is suitable.Tradition is measured polyether glycol hydroxyl value and is carried out according to < < State Standard of the People's Republic of China > > GB12008.3-89; it is acylating reagent that the method adopts phthalic anhydride; the concentrated sulphuric acid is catalyzer; in the oil bath pan of 85 ℃ under counterflow condition; hydroxyl be dissolved in the phthalic anhydride generation esterification in pyridine; the standard solution of sodium hydroxide titration of excessive phthalic anhydride, the key reaction of its generation is as follows:
Acidylate: alcohol and excessive phthalic anhydride generate ester and acid;
Hydrolysis: add the phthalic anhydride of water hydrolysed residual, make it generate acid;
Neutralization: use in NaOH and the acid of producing.
The method great advantage is that existing of phenol and aldehyde is noiseless, and stable reagent is non-volatile, has a small amount of water noiseless.But; the acidylate ability of the method is poor; in high molecular polyether course of reaction; occur that reaction not exclusively; the phenomenons such as response sample muddiness, have strengthened the difficulty that judges titration end-point, make phthalic acid anhydride acylation method measure hydroxyl value inaccurate; error is larger, even larger to different operator's operate misss.In addition, also can there is acylation reaction, interference measurement in primary, secondary amine and mercaptan.
Summary of the invention
The shortcoming existing for above-mentioned existing standard, the invention provides a kind of method of measuring alcohol hydroxyl value, and the method is accurate, simple to operate, efficient, avoids the pyridine that uses stench poisonous, has the advantages such as interference of eliminating primary, secondary amine in polyether glycol simultaneously.
Technical matters to be solved by this invention is to provide a kind of method of measuring alcohol hydroxyl value.The method comprises the following steps:
A, acylation reaction: accurately take a certain amount of sample, add anhydrous sodium acetate, add excessive acetic anhydride, after whole reaction system reaches 83～87 ℃, continue reaction 5～10min, stop reaction;
B, hydrolysis reaction: add distilled water, continue to be heated to boiling, fully reaction, is cooled to room temperature;
C, neutralization reaction: add phenolphthalein indicator, with aqueous slkali, be neutralized to neutrality;
D, saponification: accurately add excessive aqueous slkali, after ebuillition of heated, continue heating 8～10min, be cooled to room temperature;
E, titration: with acid solution, be titrated to terminal, record the volume V of consumption acids solution;
F, blank test: use the same method and do blank test, record the volume V of consumption acids solution
0;
G, experimental result are calculated:
In formula: x-hydroxyl value, mgKOH/g;
M-the take quality of sample, g;
V
0the consumption of acid solution during-blank titration, mL;
The consumption of acid solution during the titration of V-sample, mL;
Hydrionic concentration in C-acid solution, mol/L;
The molal weight of 56.1-potassium hydroxide, g/mol.
Concrete, in said method, described sample is any one in dibasic alcohol, trihydroxy alcohol or tetra-atomic alcohol.
Preferably, in said method, described molecular weight analyte≤500 o'clock, the sample quality taking is 0.1～0.8g; 500 < molecular weight≤5000 o'clock, the sample quality taking is 3.0～4.0g.
Preferably, in said method, the mol ratio of sample and sodium acetate is 0.1～1.1 ︰ 1.
Preferably, in said method, the mol ratio of acetic anhydride and sample is 4～22 ︰ 1.
Preferably, in said method, in steps d, described aqueous slkali is any one in sodium hydrate aqueous solution or potassium hydroxide aqueous solution.
Further preferred, in said method, the NaOH in described sodium hydrate aqueous solution or the mol ratio of the potassium hydroxide in potassium hydroxide aqueous solution and sample are 3～15 ︰ 1.
Further preferred, in said method, described sodium hydrate aqueous solution or potassium hydroxide aqueous solution concentration are 0.4～0.6mol/L.
Preferably, in said method, described acid solution is hydrochloric acid.
Further preferred, in said method, described concentration of hydrochloric acid is 0.4～0.6mol/L.
The present invention adopts acetic anhydride-sodium acetate to measure the method for hydroxyl value in alcohol, applied range, not only can measure the hydroxyl value of polyvalent alcohol in little molecule (as ethylene glycol, glycerine, trimethylolpropane and pentaerythrite etc.), and can measure the polyethers of high molecular containing the hydroxyl value of energy bonding agent (as GAP, BAMO and AMMO etc.); The inventive method can be eliminated the interference of primary, secondary amine simultaneously, simple to operate, measurement result accurately, quick, error is little, there is higher accuracy and reappearance simultaneously, and, the method is avoided the pyridine that uses stench poisonous, little to the harm of human body and environment, and the mensuration that the inventive method is hydroxyl value in alcohol provides a better selection approach.
Embodiment
A method of measuring alcohol hydroxyl value, comprises the following steps:
A, acylation reaction: accurately take a certain amount of sample, add anhydrous sodium acetate, add excessive acetic anhydride, after whole reaction system reaches 83～87 ℃, continue reaction 5～10min, stop reaction;
B, hydrolysis reaction: add distilled water, continue to be heated to boiling, fully reaction, is cooled to room temperature;
C, neutralization reaction: add phenolphthalein indicator, with aqueous slkali, be neutralized to neutrality;
D, saponification: accurately add excessive aqueous slkali, after ebuillition of heated, continue heating 8～10min, be cooled to room temperature;
E, titration: with acid solution, be titrated to terminal, record the volume V of consumption acids solution;
F, blank test: use the same method and do blank test, record the volume V of consumption acids solution
0;
G, experimental result are calculated:
In formula: x-hydroxyl value, mgKOH/g;
M-the take quality of sample, g;
V
0the consumption of acid solution during-blank titration, mL;
The consumption of acid solution during the titration of V-sample, mL;
Hydrionic concentration in C-acid solution, mol/L;
The molal weight of 56.1-potassium hydroxide, g/mol.
Concrete, described sample is any one in dibasic alcohol, trihydroxy alcohol or tetra-atomic alcohol.
Preferably, in order to make measurement result accurately and reliably, do not waste raw material again, when described molecular weight analyte≤500, the sample quality taking is 0.1～0.8g simultaneously; When 500 < molecular weight≤5000, the sample quality taking is 3.0～4.0g.
Preferably, the mol ratio of sample and sodium acetate is 0.1～1.1 ︰ 1.
Preferably, for make acetic anhydride can be completely and sample react, acetic anhydride should be excessive; Further, for measurement result is not accurately wasted again acetic anhydride, preferably the mol ratio of acetic anhydride and sample is 4～22 ︰ 1.
Preferably, in order to make the ester of aqueous slkali and generation fully saponified, aqueous slkali should be excessive.Preferred bases solution is any one in sodium hydrate aqueous solution or potassium hydroxide aqueous solution.Further, for measurement result does not accurately waste raw material again, preferably the NaOH in sodium hydrate aqueous solution or the mol ratio of the potassium hydroxide in potassium hydroxide aqueous solution and sample are 3～15 ︰ 1.Preferably the concentration of sodium hydrate aqueous solution or potassium hydroxide aqueous solution is 0.4～0.6mol/L.
Preferably, described acid solution is hydrochloric acid.Further preferred, described concentration of hydrochloric acid is 0.4～0.6mol/L.
Alcohol hydroxyl value of the present invention refers to milligram number, the i.e. mgKOH/g of the potassium hydroxide that the hydroxyl in 1g sample is suitable.
The inventive method be take acetic anhydride as acylating reagent, and sodium acetate is catalyzer, and alcohol and acetic anhydride generation esterification generate ester and acetic acid; excessive acetic anhydride adds water makes its hydrolysis generate acetic acid; with in aqueous slkali and acetic acid, then add excessive aqueous slkali, make ester generation saponification.After having reacted, with the remaining alkali of acid solution titration; Carry out under the same conditions blank test, the difference of blank test and sample consumption acids solution is the alkali that ester generation saponification consumes, thereby calculates hydroxy radical content.
Take GAP during as example, and the related reaction equation of the inventive method is as follows:
(1) acidylate: GAP and excessive acetic anhydride react and generate ester and acetic acid, and reaction equation is as follows:
In the inventive method, acetic anhydride and alcohol react and generate ester and acetic acid, and for alcohol being reacted completely, acetic anhydride is excessive, but in order not waste acetic anhydride, the mol ratio of acetic anhydride and alcohol can be controlled is 4～22 ︰ 1.
(2) hydrolysis: add the acetic anhydride of water hydrolysed residual, make it generate acetic acid, reaction equation is as follows:
(3) neutralization: use in aqueous slkali and the acid of producing, reaction equation is as follows:
CH
3COOH+NaOH→CH
3COONa+H2O
(4) saponification: add the ester generation saponification of excessive aqueous slkali and generation, reaction equation is as follows:
In the inventive method, the ester generation saponification of aqueous slkali and generation herein, for ester being reacted completely, aqueous slkali should be excessive, in order not waste too much aqueous slkali and acid solution, preferably by aqueous slkali and sample mol ratio to control be 3～15 ︰ 1, the concentration of aqueous slkali is 0.4～0.6mol/L.
Saponification of the present invention adds after aqueous slkali, owing to there being the existence of phenolphthalein reagent, the aobvious pink of solution, when if the aqueous slkali amount adding when saponification is inadequate, after reaction, solution is aobvious colourless, the aobvious pink of solution after saponification now can add aqueous slkali to react, until can be carried out next step titration and be detected again.The amount of the aqueous slkali adding of this step should precise record, to add the aqueous slkali of same amount when doing blank test.
(5) titration: with the remaining alkali of acidometric titration solution, reaction equation is as follows:
HCl+NaOH→NaCl+H
2O
Below in conjunction with embodiment, the present invention is described in further detail, in the embodiment of the present invention 1～5, molecular weight adopts gel permeation chromatography (GPC) to measure, and functionality is by calculating.
Embodiment 1 measures the hydroxyl value of PEG1000
Take PEG1000 sample 3.4571g and be placed in 500ml conical flask (can not allow sample contact with bottleneck), add 0.35g anhydrous sodium acetate; With pipette, extract 2mL acetic anhydride, be added to and claim to have in the conical flask of sample, while making system temperature be 85 ± 2 ℃ with constant-temperature heating magnetic stirring apparatus, continue heating 5～10min, add 25mL distilled water, continue to be heated to boiling, constantly shake, make solution as clear as crystal; Take off round-bottomed flask, be cooled to room temperature, add 0.5mL phenolphthalein indicator (3～5), with 0.5061mol/L standard solution of sodium hydroxide, be neutralized to blush, the 0.5061mol/L sodium hydroxide solution (in order to prevent that bumping can addend grain beaded glass) that accurately adds again 30mL, ebuillition of heated 10min, be cooled to rapidly room temperature, add 0.5mL phenolphthalein indicator (3～5), with 0.5018mol/L hydrochloric acid standard solution, be titrated to terminal, the volume V of record standard hydrochloric acid consumption is 16.38mL.
With same method, do blank test, blank test hydrochloric acid consumes volume V
0for 30.08mL, according to hydroxyl value computing formula
the hydroxyl value of PEG1000 is 111.56mgKOH/g.Number-average molecular weight is 1000, and the functionality f that obtains thus PEG1000 is 1.99, approaches the theoretical functionality (fexo is 2.0) of PEG1000.
Embodiment 2 measures the hydroxyl value of PEG2000
Take PEG2000 sample 3.3684g and be placed in 500ml conical flask (can not allow sample contact with bottleneck), add 0.35g anhydrous sodium acetate; With pipette, extract 2mL acetic anhydride, be added to and claim to have in the conical flask of sample, while making system temperature be 85 ± 2 ℃ with constant-temperature heating magnetic stirring apparatus, continue heating 5～10min, add 25ml distilled water, continue to be heated to boiling, constantly shake, make solution as clear as crystal.Take off conical flask, be cooled to room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5061mol/L standard solution of sodium hydroxide, be neutralized to blush, the 0.5061mol/L sodium hydroxide solution (in order to prevent that bumping can addend grain beaded glass) that accurately adds again 30ml, ebuillition of heated 10min, be cooled to rapidly room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5018mol/L hydrochloric acid standard solution, be titrated to terminal, the volume V of record standard hydrochloric acid consumption is 22.94mL.
With same method, do blank test, blank test hydrochloric acid consumes volume V
0for 29.95mL.According to hydroxyl value computing formula
the hydroxyl value of PEG2000 is 58.58mgKOH/g.PEG2000 number-average molecular weight is 2000, and the functionality f that obtains thus PEG2000 is 2.08, close to the theoretical functionality (fexo is 2.0) of PEG2000.
Embodiment 3 measures the hydroxyl value of GAP
Take GAP sample 3.4631g and be placed in 500ml conical flask (can not allow sample contact with bottleneck), add 0.35g anhydrous sodium acetate; With pipette, extract 2mL acetic anhydride, be added to and claim to have in the conical flask of sample, while making system temperature be 85 ± 2 ℃ with constant-temperature heating magnetic stirring apparatus, continue heating 5～10min, add 25ml distilled water, continue to be heated to boiling, constantly shake, make solution as clear as crystal.Take off conical flask, be cooled to room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5061mol/L standard solution of sodium hydroxide, be neutralized to blush, the 0.5061mol/L sodium hydroxide solution (in order to prevent that bumping can addend grain beaded glass) that accurately adds again 30ml, ebuillition of heated 10min, be cooled to rapidly room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5018mol/L hydrochloric acid standard solution, be titrated to terminal, the volume V of record standard hydrochloric acid consumption is 25.14mL.
With same method, do blank test, blank test hydrochloric acid consumes volume V
0for 29.98mL.According to hydroxyl value computing formula
the hydroxyl value of GAP is 39.34mgKOH/g.GAP number-average molecular weight is 2871, and the functionality f that obtains thus GAP is 2.01.
Embodiment 4 measures the hydroxyl value of glycerine
Take glycerine 0.1558g and be placed in 500ml conical flask (can not allow sample contact with bottleneck), add 0.35g anhydrous sodium acetate; With pipette, extract 2mL acetic anhydride, be added to and claim to have in the conical flask of sample, while making system temperature be 85 ± 2 ℃ with constant-temperature heating magnetic stirring apparatus, continue heating 5～10min, add 25ml distilled water, continue to be heated to boiling, constantly shake, make solution as clear as crystal.Take off conical flask, be cooled to room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5061mol/L standard solution of sodium hydroxide, be neutralized to blush, more accurately add the 0.5061mol/L sodium hydroxide solution (in order to prevent that bumping can addend grain beaded glass) of 30ml, boiling 10min, be cooled to rapidly room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5018mol/L hydrochloric acid standard solution, be titrated to terminal, the volume V that record standard hydrochloric acid consumes.The volume that records consumption hydrochloric acid is 20.02mL.
With same method, do blank test, blank test hydrochloric acid consumes volume V
0for 30.00mL.According to hydroxyl value computing formula
the hydroxyl value of glycerine is 1810.79mgKOH/g.Glycerine molecular weight is 92.09, and the functionality f that obtains thus glycerine is 2.97, approaches the theoretical functionality (fexo is 3.0) of glycerine.
Embodiment 5 measures the hydroxyl value of triethylene-glycol
Take triethylene-glycol 0.6911g and be placed in 500ml conical flask (can not allow sample contact with bottleneck), add 0.35g anhydrous sodium acetate; With pipette, extract 2mL acetic anhydride, be added to and claim to have in the conical flask of sample, while making system temperature be 85 ± 2 ℃ with constant-temperature heating magnetic stirring apparatus, continue heating 5～10min, add 25ml distilled water, continue to be heated to boiling, constantly shake, make solution as clear as crystal.Take off conical flask, be cooled to room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5061mol/L standard solution of sodium hydroxide, be neutralized to blush, more accurately add the 0.5061mol/L sodium hydroxide solution (in order to prevent that bumping can addend grain beaded glass) of 40ml, ebuillition of heated 10min, be cooled to rapidly room temperature, add 0.5ml phenolphthalein indicator (3～5), with 0.5058mol/L hydrochloric acid standard solution, be titrated to terminal, the volume V that record standard hydrochloric acid consumes.The volume that records consumption hydrochloric acid is 20.09mL.
With same method, do blank test, blank test hydrochloric acid consumes volume V
0for 39.23mL.According to hydroxyl value computing formula
the hydroxyl value of triethylene-glycol is 752.60mgKOH/g.Triethylene-glycol molecular weight is 150.18, and the functionality f that obtains thus triethylene-glycol is 2.01, approaches the theoretical functionality (fexo is 2.0) of triethylene-glycol.
Table 1 acetic anhydride-sodium acetate method is measured hydroxyl value
Table 2PEG hydroxy value measuring result
Repeat the operation steps of embodiment 3, record the parallel experiment result of hydroxyl value in GAP, as follows:
Table 3GAP hydroxy value measuring result
As can be seen from Table 3, the hydroxyl value standard deviation that the inventive method is measured is little, and accuracy is high, favorable reproducibility.And the hydroxyl value result that national military standard phthalic anhydride method determines and notional result error are larger; hydroxyl value performance that can not actual response sample; cause functionality resultant error large, this is because phthalic acid anhydride acylation ability is poor, with example reaction not exclusively due to.
In summary it can be seen, the hydroxyl value result that the inventive method determines and theoretical hydroxyl value approach, and its error is very little; Applied range, not only can measure the hydroxyl value of polyvalent alcohol in little molecule (as ethylene glycol, glycerine, trimethylolpropane and pentaerythrite etc.), and can measure the polyethers of high molecular containing the hydroxyl value of energy bonding agent (as GAP, BAMO and AMMO etc.); The inventive method can be eliminated the interference of primary, secondary amine simultaneously, simple to operate, measurement result accurately, quick, error is little, there is higher accuracy and reappearance, and, the method is avoided the pyridine that uses stench poisonous, little to the harm of human body and environment, and the mensuration that the inventive method is hydroxyl value in alcohol provides a better selection approach.
Claims (10)
1. a method of measuring alcohol hydroxyl value, is characterized in that: comprise the following steps:
A, acylation reaction: accurately take a certain amount of sample, add anhydrous sodium acetate, add excessive acetic anhydride, after whole reaction system reaches 83～87 ℃, continue reaction 5～10min, stop reaction;
B, hydrolysis reaction: add distilled water, continue to be heated to boiling, fully reaction, is cooled to room temperature;
C, neutralization reaction: add phenolphthalein indicator, with aqueous slkali, be neutralized to neutrality;
D, saponification: accurately add excessive aqueous slkali, after ebuillition of heated, continue heating 8～10min, be cooled to room temperature;
E, titration: with acid solution, be titrated to terminal, record the volume V of consumption acids solution;
F, blank test: use the same method and do blank test, record the volume V of consumption acids solution
0;
G, experimental result are calculated:
In formula: x-hydroxyl value, mgKOH/g;
M-the take quality of sample, g;
V
0the consumption of acid solution during-blank titration, mL;
The consumption of acid solution during the titration of V-sample, mL;
Hydrionic concentration in C-acid solution, mol/L;
The molal weight of 56.1-potassium hydroxide, g/mol.
2. method according to claim 1, is characterized in that: described sample is any one in dibasic alcohol, trihydroxy alcohol or tetra-atomic alcohol.
3. method according to claim 1 and 2, is characterized in that: described molecular weight analyte≤500 o'clock, and the sample quality taking is 0.1～0.8g; 500 < molecular weight≤5000 o'clock, the sample quality taking is 3.0～4.0g.
4. method according to claim 1 and 2, is characterized in that: the mol ratio of sample and sodium acetate is 0.1～1.1 ︰ 1.
5. method according to claim 1 and 2, is characterized in that: the mol ratio of acetic anhydride and sample is 4～22 ︰ 1.
6. method according to claim 1 and 2, is characterized in that: described aqueous slkali is any one in sodium hydrate aqueous solution or potassium hydroxide aqueous solution.
7. method according to claim 6, is characterized in that: in steps d, the NaOH in sodium hydrate aqueous solution or the mol ratio of the potassium hydroxide in potassium hydroxide aqueous solution and sample are 3～15 ︰ 1.
8. method according to claim 6, is characterized in that: in steps d, described sodium hydrate aqueous solution or potassium hydroxide aqueous solution concentration are 0.4～0.6mol/L.
9. method according to claim 1 and 2, is characterized in that: described acid solution is hydrochloric acid.
10. method according to claim 9, is characterized in that: described concentration of hydrochloric acid is 0.4～0.6mol/L.
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