CN102768263B - The assay method of pentaerythrite solution concentration in a kind of production of polyester - Google Patents

The assay method of pentaerythrite solution concentration in a kind of production of polyester Download PDF

Info

Publication number
CN102768263B
CN102768263B CN201210254287.1A CN201210254287A CN102768263B CN 102768263 B CN102768263 B CN 102768263B CN 201210254287 A CN201210254287 A CN 201210254287A CN 102768263 B CN102768263 B CN 102768263B
Authority
CN
China
Prior art keywords
pentaerythrite
solution
concentration
density
polyester
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201210254287.1A
Other languages
Chinese (zh)
Other versions
CN102768263A (en
Inventor
瞿振清
沈向东
罗厚忠
师百同
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Changle Fiber S & T Co ltd
Original Assignee
Jiangsu Changle Fiber S & T Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Changle Fiber S & T Co ltd filed Critical Jiangsu Changle Fiber S & T Co ltd
Priority to CN201210254287.1A priority Critical patent/CN102768263B/en
Publication of CN102768263A publication Critical patent/CN102768263A/en
Application granted granted Critical
Publication of CN102768263B publication Critical patent/CN102768263B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The present invention relates to the analytical approach of pentaerythrite solution concentration in a kind of production of polyester, the method comprises the configuration of normal concentration solution and the mensuration of normal concentration solution density, the step such as content of pentaerythrite in the pentaerythrite solution finally added according to formulae discovery polyester device.The present invention, according to the density of solution and solution concentration this principle linear, utilizes the method setting up density-concentration typical curve relation, achieves quick, the Accurate Determining of the pentaerythrite concentration of adding in production of polyester.

Description

The assay method of pentaerythrite solution concentration 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
Need to add titania as matting agent in production of polyester, antimony glycol, as catalyzer, also been developed another kind of A type adjuvant in recent years.A type adjuvant formal name used at school pentaerythrite (PER), white crystals or powder, relative density: 1.395g/cm3, fusing point: 261 ~ 262 DEG C, boiling point: 276 DEG C, is dissolved in the organic solvents such as ethanol, glycerine, ethylene glycol, formamide.It is mainly for the manufacture of alkyd resin and paint, manufactures stabilizer for plastics and plastifier, and for the manufacture of nitropenthrite detonating powder etc.In view of A type adjuvant has the effect of stabilizer for plastics and plastifier, add the spinning properties that A type adjuvant can increase fiber, be conducive to the stable of aft-loaded airfoil, and be soluble in the feature of ethylene glycol, can in fiber-grade polyester process units, A type adjuvant and ethylene glycol are mixed with the solution that massfraction is 4%, then add PTA slurry preparation, participate in esterification and polycondensation reaction.
Therefore, the mensuration of its actual concentrations in A type adjuvant process for preparation is seemed be even more important.But, A type additive concentration is measured there is no authority, accurately assay method at present.
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, according to the density of solution and solution concentration this principle linear, utilizes the method setting up density-concentration typical curve relation, can carry out the Accurate Determining of pentaerythrite solution concentration.
In order to realize foregoing invention object, the technical solution used in the present invention is as follows:
An analytical approach for pentaerythrite solution concentration in production of polyester, comprising:
Step 1: the configuration of normal concentration solution and density measurement, it comprises the following steps:
1) take pentaerythrite as solute, ethylene 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 pentaerythrite solution of polyester device preparation;
2) density of bioassay standard concentration pentaerythrite solution;
3) according to the linear relationship between the massfraction of normal concentration pentaerythrite solution and density, the slope K in linear function y=Kx+b is determined;
Step 2: the mensuration of pentaerythrite content in the pentaerythrite solution of polyester device preparation, it comprises the following steps:
1) polyester device take pentaerythrite as solute, and ethylene glycol is solvent, preparation pentaerythrite solution;
2) measure the density of preparation pentaerythrite solution ethylene glycol used, many surveys several times, get its mean value ρ 1; Measure the quality m of empty iodine flask 1;
3) ethylene glycol having measured density is placed in sky iodine flask, measures the quality m of the iodine flask after splendid attire ethylene glycol 2, being wherein placed in the volume of the ethylene glycol of iodine flask with the ratio of the volume of iodine flask is 1:3 ~ 1:2;
4) in the iodine flask that ethylene glycol is housed, add the pentaerythrite solution of above-mentioned polyester device preparation and mix, obtain mixed solution, the volume of pentaerythrite solution wherein added is 1:5 ~ 1:3 with the ratio of the volume of iodine flask;
5) the quality m that the iodine flask of mixed solution is housed is measured 3and the density p of mixed solution 2;
6) according to the concentration C of the pentaerythrite solution of following formulae discovery polyester device preparation:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 % .
In an embodiment of the present invention, in step 2, the pentaerythrite solution that above-mentioned polyester device is prepared before adding the iodine flask that ethylene glycol is housed first to carrying out discharge opeing in polyester device pipeline until flow out pentaerythrite solution temperature reach more than 70 DEG C.
In an embodiment of the present invention, the density of densitometer to ethylene glycol solution, mixed solution with heat insulation function is utilized to measure.
In an embodiment of the present invention, densitometric sample heat-insulation unit temperature is set as 50 ~ 70 DEG C, and densimeter measurement temperature is set as 15 ~ 25 DEG C.
In an embodiment of the present invention, densitometer is before measuring first with air and pure water calibration.If the Density Calibration result of air and pure water goes beyond the scope, clean and dry density meter U-shaped pipe with the pure absolute ethyl alcohol of analysis and acetone respectively.
Accompanying drawing explanation
Fig. 1 pentaerythrite concentration and density criterion curve.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but and unrestricted range of application of the present invention.
The present invention's density used counts 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 ethylene glycol is technical grade, high-class product, and pentaerythrite is industrial pentaerythrite, 98 grades.
The principle of embodiment 1 computing formula and derivation
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, when showing low concentration pentaerythrite solution (being less than 4.5%) density and its concentration linear, utilize this typical curve can derive the actual concentrations of the pentaerythrite solution of polyester device preparation.
Formula proving of the present invention is as follows:
1. defining according to straight slope
K=(ρ 2-ρ 1)/(C 2-C 1) formula (1)
Wherein ρ 2, C 2represent density and the concentration of the mixed solution that the pentaerythrite solution that ethylene glycol and polyester device are prepared is formed;
ρ 1, C 1represent density and the concentration (C of neat solvent ethylene glycol 1=0);
2. according to the step 2 in summary of the invention
C 2=Solute mass [C × (m 3-m 2)]/solution quality [(m 3-m 1)] × 100% formula (2)
C wherein represents the massfraction of the pentaerythrite solution that polyester device is prepared;
Derived by above-mentioned formula (1) and (2) and obtain the concentration computing formula of the pentaerythrite solution that polyester device is prepared:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 % .
The preparation of embodiment 2 normal concentration solution and density measurement
With pentaerythrite as solute, ethylene glycol, as solvent, is prepared one group of massfraction and is respectively: 2.50%, the normal concentration solution of 3.00%, 3.50%, 4.00%, 4.50%, measures the density value of this group solution.
Actual preparation pentaerythrite concentration and density measurement result as follows:
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
As shown in Figure 1, wherein y-axis represents density, and x-axis represents concentration for pentaerythrite concentration and density criterion curve.
Can obtain y=0.1697x+1.1129 thus, the K namely in linear function y=Kx+b is 0.1697.
The concentration determination of embodiment 3 pentaerythrite sample 1
Polyester device take pentaerythrite as solute, and ethylene glycol is solvent, the solution of preparation pentaerythrite sample 1.During preparation, analyst gets the solution of preparation pentaerythrite sample 1 ethylene glycol used to scene.
Its three density of replicate determination after laboratory fetched by ethylene glycol the ρ that averages 1=1.11341g/cm 3;
The quality record taking sky iodine flask (volume 150ml) is m 1=112.3485g;
Add 60g(and be about 55ml) ethylene glycol fetched in iodine flask, the quality m of record iodine flask and ethylene glycol 2=174.2302g;
Before the about 35ml(of solution of the pentaerythrite sample 1 iodine flask scene of taking weighing up ethylene glycol being added polyester device preparation adds first to carrying out discharge opeing in polyester device pipeline until the pentaerythrite solution temperature flowed out reaches more than 70 DEG C) to iodine flask scale mark about 90ml, in time the iodine flask that mixed solution is housed is brought back laboratory and weighs its quality m 3=214.4868g;
The density of mixed solution is measured with densitometer and to record result be ρ after stirring 2=1.11603(g/cm 3);
Concentration according to following formulae discovery pentaerythrite:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 %
In formula: m 1for the quality of iodine flask
M 2for the quality of iodine flask and ethylene glycol
M 3for the quality of mixed solution and iodine flask
K=0.1697 is the slope of typical curve
Calculate C=3.92%.
In mensuration process, densitometer sample heat-insulation unit temperature is set as 60 DEG C, and densimeter measurement temperature is set as 20 DEG C;
First with air and pure water calibration before densimeter measurement:
Air (20 DEG C) density: 0.0012 ± 0.0001g/cm 3
Pure water (20 DEG C) density: 0.9982 ± 0.0001g/cm 3
If the Density Calibration result of air and pure water goes beyond the scope, respectively with analyzing the clean and dry density meter U-shaped pipe of pure absolute ethyl alcohol and acetone, calibrate qualified after can measure ethylene glycol and pentaerythrite mixed solution density.
The concentration determination of embodiment 4 ~ 8 pentaerythrite sample 2 ~ 6
Concrete operation step is with embodiment 3.
Measurement result is as shown in table 1 below.
Table 1
The foregoing is only preferred embodiment of the present invention, be not used for limiting practical range of the present invention; If do not depart from the spirit and scope of the present invention, the present invention is modified or equivalent to replace, in the middle of the protection domain that all should be encompassed in the claims in the present invention.

Claims (4)

1. the analytical approach of pentaerythrite solution concentration in production of polyester, is characterized in that, comprising:
Step 1: the configuration of normal concentration solution and density measurement, it comprises the following steps:
1) take pentaerythrite as solute, ethylene 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 pentaerythrite solution of polyester device preparation;
2) density of bioassay standard concentration pentaerythrite solution;
3) according to the linear relationship between the massfraction of normal concentration pentaerythrite solution and density, the slope K in linear function y=Kx+b is determined, in formula: y represents density, g/cm 3; X represents concentration, wt%; B represents intercept;
Step 2: the mensuration of pentaerythrite content in the pentaerythrite solution of polyester device preparation, it comprises the following steps:
1) polyester device take pentaerythrite as solute, and ethylene glycol is solvent, preparation pentaerythrite solution;
2) utilize the densitometer with heat insulation function to measure the density of preparation pentaerythrite solution ethylene glycol used, many surveys several times, get its mean value ρ 1; Wherein, densitometer is before measuring first with air and pure water calibration; Densitometric sample heat-insulation unit temperature is set as 50 ~ 70 DEG C; Measure the quality m of empty iodine flask 1;
3) ethylene glycol having measured density is placed in sky iodine flask, measures the quality m of the iodine flask after splendid attire ethylene glycol 2, being wherein placed in the volume of the ethylene glycol of iodine flask with the ratio of the volume of iodine flask is 1:3 ~ 1:2;
4) in the iodine flask that ethylene glycol is housed, add the pentaerythrite solution of above-mentioned polyester device preparation and mix, obtain mixed solution, the volume of pentaerythrite solution wherein added is 1:5 ~ 1:3 with the ratio of the volume of iodine flask;
5) densitometer with heat insulation function is utilized to measure the quality m that the iodine flask of mixed solution is housed 3and the density p of mixed solution 2; Wherein, densitometer is before measuring first with air and pure water calibration; Densitometric sample heat-insulation unit temperature is set as 50 ~ 70 DEG C;
6) according to the concentration C of the pentaerythrite solution of following formulae discovery polyester device preparation:
C = ρ 2 - ρ 1 K × m 3 - m 1 m 3 - m 2 × 100 % .
2. the analytical approach of pentaerythrite solution concentration in production of polyester according to claim 1, it is characterized in that, in step 2, the pentaerythrite solution that above-mentioned polyester device is prepared before adding the iodine flask that ethylene glycol is housed first to carrying out discharge opeing in polyester device pipeline until flow out pentaerythrite solution temperature reach more than 70 DEG C.
3. the analytical approach of pentaerythrite solution concentration in production of polyester according to claim 1, it is characterized in that, densimeter measurement temperature is set as 15 ~ 25 DEG C.
4. the analytical approach of pentaerythrite solution concentration in production of polyester according to claim 1, is characterized in that, if the Density Calibration result of air and pure water goes beyond the scope, respectively with analyzing pure absolute ethyl alcohol and acetone is clean and dry density meter U-shaped pipe.
CN201210254287.1A 2012-07-23 2012-07-23 The assay method of pentaerythrite solution concentration in a kind of production of polyester Active CN102768263B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210254287.1A CN102768263B (en) 2012-07-23 2012-07-23 The assay method of pentaerythrite solution concentration in a kind of production of polyester

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210254287.1A CN102768263B (en) 2012-07-23 2012-07-23 The assay method of pentaerythrite solution concentration in a kind of production of polyester

Publications (2)

Publication Number Publication Date
CN102768263A CN102768263A (en) 2012-11-07
CN102768263B true CN102768263B (en) 2015-08-12

Family

ID=47095736

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210254287.1A Active CN102768263B (en) 2012-07-23 2012-07-23 The assay method of pentaerythrite solution concentration in a kind of production of polyester

Country Status (1)

Country Link
CN (1) CN102768263B (en)

Families Citing this family (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
CN111272608B (en) * 2020-03-19 2021-04-02 南京正大天晴制药有限公司 Content determination method of stable nonionic 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

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1815190A (en) * 2006-02-20 2006-08-09 扬州大学 Method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1815190A (en) * 2006-02-20 2006-08-09 扬州大学 Method for determining styrene micro-emulsion polymerization conversion rate by ultraviolet spectrometry
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
聚酯熔体中添加季戊四醇的研究;辛东坡;《合成纤维》;20111231(第5期);全文 *

Also Published As

Publication number Publication date
CN102768263A (en) 2012-11-07

Similar Documents

Publication Publication Date Title
CN102768263B (en) The assay method of pentaerythrite solution concentration in a kind of production of polyester
CN103512829A (en) Method for measuring sediment concentration through density of muddy water
CN106153498A (en) A kind of new method detecting solute concentration in solution and device thereof
CN107505348A (en) Application of the metronidazole as internal standard compound in hydrogen nuclear magnetic resonance technology
Ivashchenko et al. Application of the sorption-frequency method in comparison with other methods for measurement of humidity nanoconcentrations in gases and liquids
CN105301031B (en) The method that one-dimensional nuclear magnetic resonance hydrogen spectrometry determines containing hydrogen silicone oil residual quantity in trisiloxane surfactant
CN102608246A (en) Method for determining water content in glyceryl triacetate
CN106442342B (en) A kind of method of sulfur trioxide and sulfuric acid concentration in measurement workplace air
CN108490110A (en) A kind of method of the high containing hydrogen silicone oil hydrogen content of rapid and accurate determination
CN112844217A (en) Preparation method of dicofol standard solution
CN101329269A (en) Method for determining concentration of single ingredient water solution with known solute
CN102854264B (en) Method for determining methanol content and methyl acetate content in polyvinyl alcohol
CN105928856B (en) A kind of biomass carbon material absorption property rapid detection method
CN105424642A (en) Method for measuring content of alkyl groups or alkoxy groups in polysiloxane
Makishima et al. The Viscosity and Thermal Stability of Vapor of Trimethyl Borate
CN103162998A (en) Manufacturing method of uranium dioxide-gadolinium oxide pellet standard substance
CN106596324A (en) Method for conveniently and fast measuring content of organic acid and bamboo tar in bamboo vinegar
CN106124547A (en) A kind of measure the method for potassium content in industrial potassium nitrate
Ananthanarayanan et al. High resolution conductometry for isotopic assay of deuterium in mixtures of heavy water and light water
CN105675809A (en) Analysis method of concentration of HI-I2-H2O ternary solution
CN102841035A (en) Alcohol base fuel heating value measurement technology
Resler et al. Accuracy and Precision of Portable Turbidity Meters
CN104568644A (en) Method for measuring content of sand in water sample by use of 1000ml volumetric flask
CN111272684A (en) Fe in electrolyte2+Method for measuring concentration
Anghel et al. Quality Assurance of Breath Alcohol Measurements

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant