CN102768263A - Method for measuring concentration of pentaerythritol solution in polyester production - Google Patents

Method for measuring concentration of pentaerythritol solution in polyester production Download PDF

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CN102768263A
CN102768263A CN2012102542871A CN201210254287A CN102768263A CN 102768263 A CN102768263 A CN 102768263A CN 2012102542871 A CN2012102542871 A CN 2012102542871A CN 201210254287 A CN201210254287 A CN 201210254287A CN 102768263 A CN102768263 A CN 102768263A
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solution
pentaerythrite
concentration
density
polyester
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CN102768263B (en
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瞿振清
沈向东
罗厚忠
师百同
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Jiangsu Changle Fiber S & T Co ltd
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Jiangsu Changle Fiber S & T Co ltd
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Abstract

The invention relates to a method for measuring concentration of a pentaerythritol solution in polyester production. The method comprises the following steps of: preparing a standard concentration solution; measuring the density of the standard concentration solution; and finally calculating the content of pentaerythritol in the pentaerythritol solution added in a polyester device according to a formula. According to the principle of the linear relationship between the density of the solution and the concentration of the solution, a method for establishing a relationship between standard curves of the density and the concentration is utilized, so that the concentration of the pentaerythritol added in the polyester production is rapidly and accurately measured.

Description

Pentaerythrite Measurement Of The Concentration Of Solution method in a kind of production of polyester
Technical field
The present invention relates to chemical technology field, be specifically related to the analytical approach of pentaerythrite solution concentration in a kind of production of polyester.
Background technology
In production of polyester, need to add titania as matting agent, antimony glycol is as catalyzer, also develops in recent years another kind of A type adjuvant.A type adjuvant formal name used at school pentaerythrite (PER), white crystals or powder, relative density: 1.395g/cm3, fusing point: 261～262 ℃, boiling point: 276 ℃, be dissolved in organic solvents such as ethanol, glycerine, monoethylene glycol, formamide.It is mainly used in makes alkyd resin and paint, makes stabilizer for plastics and plastifier, and is used to make nitropenthrite detonating powder etc.The effect of stabilizer for plastics and plastifier is arranged in view of A type adjuvant; Adding A type adjuvant can increase the spinning properties of fiber, helps the stable of back processing, and is soluble in the characteristics of monoethylene glycol; Can be in the fiber-grade polyester process units; It is 4% solution that A type adjuvant and monoethylene glycol are mixed with massfraction, adds PTA slurry preparing tank then, participates in esterification and polycondensation reaction.
Therefore, the mensuration of its accurate concentration in the A type adjuvant process for preparation is seemed be even more important.Yet, at present A type additive concentration is measured do not have authority, assay method accurately.
Summary of the invention
The object of the present invention is to provide the analytical approach of pentaerythrite solution concentration in a kind of production of polyester.The present invention utilizes the method for setting up density-concentration typical curve relation according to density and linear this principle of solution concentration of solution, can carry out the accurate mensuration of pentaerythrite solution concentration.
In order to realize the foregoing invention purpose, the technical scheme that the present invention adopts is following:
The analytical approach of pentaerythrite solution concentration in a kind of production of polyester comprises:
Step 1: the configuration of normal concentration solution and density measurement, it may further comprise the steps:
1) with the pentaerythrite be solute, monoethylene glycol is solvent, and preparing one group of massfraction is W 1, W 2, W 3W nNormal concentration pentaerythrite solution, this concentration range comprises the concentration of the pentaerythrite solution of polyester device preparation;
2) density of bioassay standard concentration pentaerythrite solution;
3) according to the massfraction of normal concentration pentaerythrite solution and the linear relationship between the density, confirm the slope K among the linear function y=Kx+b;
Step 2: pentaerythrite Determination on content in the pentaerythrite solution of polyester device preparation, it may further comprise the steps:
1) polyester device is solute with the pentaerythrite, and monoethylene glycol is solvent, preparation pentaerythrite solution;
2) measure the density of preparing the used monoethylene glycol of pentaerythrite solution, survey several times got its mean value ρ more 1Measure the quality m of empty iodine flask 1
3) monoethylene glycol that will measure density places the sky iodine flask, measures the quality m of the iodine flask behind the splendid attire monoethylene glycol 2, wherein placing the ratio of volume and the volume of iodine flask of the monoethylene glycol of iodine flask is 1:3 ~ 1:2;
4) the pentaerythrite solution that the above-mentioned polyester device of adding is prepared in the iodine flask of monoethylene glycol is housed also mixes, and obtains mixed solution, and the volume of the pentaerythrite solution that wherein adds is 1:5 ~ 1:3 with the ratio of the volume of iodine flask;
5) mensuration is equipped with the quality m of the iodine flask of mixed solution 3And the density p of mixed solution 2
6) calculate the concentration C of the pentaerythrite solution of polyester device preparation according to following formula:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 % .
In an embodiment of the present invention, in the step 2, the iodine flask that the pentaerythrite solution adding of above-mentioned polyester device preparation is equipped with monoethylene glycol reaches more than 70 ℃ up to the pentaerythrite solution temperature that flows out carrying out discharge opeing in the polyester device pipeline earlier before.
In an embodiment of the present invention, utilize densitometer that the density of ethylene glycol solution, mixed solution is measured with heat insulation function.
In an embodiment of the present invention, densitometric sample heat-insulation unit temperature is set at 50 ~ 70 ℃, and the densimeter measurement temperature is set at 15 ~ 25 ℃.
In an embodiment of the present invention, densitometer is calibrated with air and pure water earlier before measurement.If the Density Calibration result of air and pure water goes beyond the scope, respectively with analyzing pure absolute ethyl alcohol and acetone cleaning and dry density meter U-shaped pipe.
Description of drawings
Fig. 1 pentaerythrite concentration and density criterion curve.
Embodiment
Below in conjunction with embodiment the present invention is described further, but and unrestricted range of application of the present invention.
The used density of the present invention is counted the DDM2911 type densitometer (carry sample heat insulation function) of RUDOLPH company, and analytical balance is the XP504 type electronic balance of METTLER company, and monoethylene glycol is technical grade, and high-class product, pentaerythrite are industrial pentaerythrite, 98 grades.
The principle and the derivation of embodiment 1 computing formula
Test the density of one group of (5) normal concentration pentaerythrite solution, be depicted as solution density and concentration relationship curve, coefficient R 2=0.9971, density and its concentration are linear when showing low concentration pentaerythrite solution (less than 4.5%), utilize this typical curve can derive the pentaerythrite accurate solution concentration of polyester device preparation.
Computing formula of the present invention is derived as follows:
1. according to defining of straight slope
K=(ρ 2-ρ 1)/(C 2-C 1) formula (1)
ρ wherein 2, C 2The density and the concentration of the mixed solution that the pentaerythrite solution of expression monoethylene glycol and polyester device preparation forms;
ρ 1, C 1The density and the concentration (C of expression neat solvent monoethylene glycol 1=0);
2. according to the step 2 in the summary of the invention
C 2=solute quality [C * (m 3-m 2)]/solution quality [(m 3-m 1)] * 100% formula (2)
C wherein representes the massfraction of the pentaerythrite solution of polyester device preparation;
Obtain the concentration computing formula of the pentaerythrite solution of polyester device preparation by above-mentioned formula (1) and (2) derivation:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 % .
The preparation and the density measurement of embodiment 2 normal concentration solution
As solute, monoethylene glycol is prepared one group of massfraction and is respectively as solvent with pentaerythrite: 3.00%, 3.50%, 4.00%, 4.50% normal concentration solution 2.50%,, measure the density value of this group solution.
Actual preparation pentaerythrite concentration and density measurement result are following:
Concentration 4.4896% 4.0521% 3.3547% 2.9824% 2.4477%
Density (g/cm 3） 1.12049 1.11982 1.11859 1.11809 1.11699
Pentaerythrite concentration and density criterion curve are as shown in Figure 1, and wherein the y axle is represented density, x axle indicated concentration.
Can obtain y=0.1697x+1.1129 thus, promptly the K among the linear function y=Kx+b is 0.1697.
The concentration determination of embodiment 3 pentaerythrite samples 1
Polyester device is solute with the pentaerythrite, and monoethylene glycol is solvent, the solution of preparation pentaerythrite sample 1.During preparation, the analyst is to the on-the-spot used monoethylene glycol of solution of getting preparation pentaerythrite sample 1.
Monoethylene glycol is fetched replicate determination its three density and ρ that averages behind the laboratory 1=1.11341g/cm 3
The quality record that takes by weighing sky iodine flask (volume 150ml) is m 1=112.3485g;
The monoethylene glycol that adding 60g (about 55ml) fetches writes down the quality m of iodine flask and monoethylene glycol in iodine flask 2=174.2302g;
The iodine flask that weighs up monoethylene glycol is taken the on-the-spot about 35ml of solution (reaching more than 70 ℃ up to the pentaerythrite solution temperature that flows out carrying out discharge opeing in the polyester device pipeline earlier before adding) that adds the pentaerythrite sample 1 of polyester device preparation to about the iodine flask scale mark 90ml, and the iodine flask that mixed solution in time will be housed is brought back its quality of laboratory weighing m 3=214.4868g;
Use densitometer to measure the density of mixed solution and write down the result after stirring and be ρ 2=1.11603 (g/cm 3);
Calculate the concentration of pentaerythrite according to following formula:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 %
In the formula: m 1Quality for iodine flask
m 2Quality for iodine flask and monoethylene glycol
m 3Quality for mixed solution and iodine flask
K=0.1697 is the slope of typical curve
Calculate C=3.92%.
In the mensuration process, densitometer sample heat-insulation unit temperature is set at 60 ℃, and the densimeter measurement temperature is set at 20 ℃;
Calibrate with air and pure water earlier before the densimeter measurement:
Air (20 ℃) density: 0.0012 ± 0.0001g/cm 3
Pure water (20 ℃) density: 0.9982 ± 0.0001g/cm 3
If the Density Calibration result of air and pure water goes beyond the scope, clean and dry density meter U-shaped pipe with acetone with analyzing pure absolute ethyl alcohol respectively, calibrate and can measure monoethylene glycol and pentaerythrite mixed solution density after qualified.
The concentration determination of embodiment 4 ~ 8 pentaerythrite samples 2 ~ 6
The concrete operations step is with embodiment 3.
Mensuration result is as shown in table 1 below.
Table 1
Figure BDA00001917737900061
The above is merely preferred embodiment of the present invention, is not to be used for limiting practical range of the present invention; If do not break away from the spirit and scope of the present invention, the present invention is made amendment or is equal to replacement, all should be encompassed in the middle of the protection domain of claim of the present invention.

Claims (7)

1. the analytical approach of pentaerythrite solution concentration in the production of polyester is characterized in that, comprising:
Step 1: the configuration of normal concentration solution and density measurement, it may further comprise the steps:
1) with the pentaerythrite be solute, monoethylene glycol is solvent, and preparing one group of massfraction is W 1, W 2, W 3W nNormal concentration pentaerythrite solution, this concentration range comprises the concentration of the pentaerythrite solution of polyester device preparation;
2) density of bioassay standard concentration pentaerythrite solution;
3) according to the massfraction of normal concentration pentaerythrite solution and the linear relationship between the density, confirm the slope K among the linear function y=Kx+b;
Step 2: pentaerythrite Determination on content in the pentaerythrite solution of polyester device preparation, it may further comprise the steps:
1) polyester device is solute with the pentaerythrite, and monoethylene glycol is solvent, preparation pentaerythrite solution;
2) measure the density of preparing the used monoethylene glycol of pentaerythrite solution, survey several times got its mean value ρ more 1Measure the quality m of empty iodine flask 1
3) monoethylene glycol that will measure density places the sky iodine flask, measures the quality m of the iodine flask behind the splendid attire monoethylene glycol 2, wherein placing the ratio of volume and the volume of iodine flask of the monoethylene glycol of iodine flask is 1:3 ~ 1:2;
4) the pentaerythrite solution that the above-mentioned polyester device of adding is prepared in the iodine flask of monoethylene glycol is housed also mixes, and obtains mixed solution, and the volume of the pentaerythrite solution that wherein adds is 1:5 ~ 1:3 with the ratio of the volume of iodine flask;
5) mensuration is equipped with the quality m of the iodine flask of mixed solution 3And the density p of mixed solution 2
6) calculate the concentration C of the pentaerythrite solution of polyester device preparation according to following formula:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 % .
2. the analytical approach of pentaerythrite solution concentration in the production of polyester according to claim 1; It is characterized in that; In the step 2, the iodine flask that the pentaerythrite solution adding of above-mentioned polyester device preparation is equipped with monoethylene glycol reaches more than 70 ℃ up to the pentaerythrite solution temperature that flows out carrying out discharge opeing in the polyester device pipeline earlier before.
3. the analytical approach of pentaerythrite solution concentration is characterized in that in the production of polyester according to claim 1 and 2, utilizes the densitometer with heat insulation function that the density of monoethylene glycol, mixed solution is measured.
4. the analytical approach of pentaerythrite solution concentration is characterized in that in the production of polyester according to claim 3, and densitometric sample heat-insulation unit temperature is set at 50 ~ 70 ℃.
5. the analytical approach of pentaerythrite solution concentration is characterized in that in the production of polyester according to claim 4, and the densimeter measurement temperature is set at 15 ~ 25 ℃.
6. the analytical approach of pentaerythrite solution concentration is characterized in that in the production of polyester according to claim 3, and densitometer is calibrated with air and pure water earlier before measurement.
7. the analytical approach of pentaerythrite solution concentration is characterized in that in the production of polyester according to claim 6, if the Density Calibration result of air and pure water goes beyond the scope, respectively with analyzing pure absolute ethyl alcohol and acetone cleaning and dry density meter U-shaped pipe.
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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN106153498A (en) * 2015-04-22 2016-11-23 中国石油化工股份有限公司 A kind of new method detecting solute concentration in solution and device thereof
CN106767936A (en) * 2017-02-09 2017-05-31 宣向斌 The concentration detection system and its detection method of a kind of use integration technology
CN110441468A (en) * 2019-05-31 2019-11-12 青岛海湾集团有限公司 The measuring method of calcium chloride solution calcium content during a kind of ammonia-soda process calcium chloride
CN111272608A (en) * 2020-03-19 2020-06-12 南京正大天晴制药有限公司 Content determination method of stable ionic iodine contrast agent
CN112504916A (en) * 2020-11-04 2021-03-16 浙江恒逸聚合物有限公司 Physical test method for rapidly determining pentaerythritol content

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CN102135486A (en) * 2010-12-22 2011-07-27 中国科学院山西煤炭化学研究所 Method for quickly detecting concentration of polyacrylonitrile-based free radical coagulation bath
CN102353606A (en) * 2011-06-13 2012-02-15 超威电源有限公司 Method for detecting distribution uniformity of colloid in colloid battery

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106153498A (en) * 2015-04-22 2016-11-23 中国石油化工股份有限公司 A kind of new method detecting solute concentration in solution and device thereof
CN106767936A (en) * 2017-02-09 2017-05-31 宣向斌 The concentration detection system and its detection method of a kind of use integration technology
CN110441468A (en) * 2019-05-31 2019-11-12 青岛海湾集团有限公司 The measuring method of calcium chloride solution calcium content during a kind of ammonia-soda process calcium chloride
CN111272608A (en) * 2020-03-19 2020-06-12 南京正大天晴制药有限公司 Content determination method of stable ionic iodine contrast agent
CN112504916A (en) * 2020-11-04 2021-03-16 浙江恒逸聚合物有限公司 Physical test method for rapidly determining pentaerythritol content

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