CN104391076A - Detection method of content of bis (3,5,5-trimethyl hexanoyl) peroxide in initiator Tx-36 - Google Patents
Detection method of content of bis (3,5,5-trimethyl hexanoyl) peroxide in initiator Tx-36 Download PDFInfo
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- CN104391076A CN104391076A CN201410607818.XA CN201410607818A CN104391076A CN 104391076 A CN104391076 A CN 104391076A CN 201410607818 A CN201410607818 A CN 201410607818A CN 104391076 A CN104391076 A CN 104391076A
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Abstract
The invention relates to the technical field of detection methods of chemical products, and relates to a detection method of content of bis (3,5,5-trimethyl hexanoyl) peroxide in an initiator Tx-36. The detection method comprises the following steps: firstly adding isopropanol, acetic acid glacial and a ferric chloride solution into an iodine flask, and uniformly mixing; then introducing nitrogen onto the liquid in the iodine flask, weighing the initiator Tx-36 and arranging the initiator Tx-36 in the iodine flask, and adding a potassium iodide solution and covering with a cork, and finally titrating with a sodium thiosulfate standard solution to be colorless. According to the method provided by the invention, isopropanol is used for replacing toxic tetrahydrofuran, the harm to laboratory personnel is alleviated, and the used ferric chloride solution is a catalyst, the detection time is greatly shortened, and a great convenience is brought to the detection work, and therefore, the results obtained by detecting the content of bis (3,5,5-trimethyl hexanoyl) peroxide in the initiator Tx-36 are relatively accurate, the operation is convenient, and the toxicity is low, so that the detection method is ideal.
Description
Technical field
the present invention relates to the detection method technical field of chemical products, is two (3,5,5-trimethyl acetyl) detection method of content of peroxidating in a kind of initiating agent Tx-36.
Background technology
polyvinylchloride, English abbreviation PVC is a kind of material of having many uses, in the life through being usually used in us, such as pvc pipe, PVC floor, PVC wallpaper etc.The demand of market to PVC increases year by year.Polyvinylchloride is one of five large general-purpose plastics.Polyvinylchloride has good mechanical property, about tensile strength 60MPa, impact strength 5 ~ 10kJ/m
2
, have excellent dielectric properties simultaneously.
the thermoplastic resin be polymerized under initiating agent effect by vinyl chloride, the namely homopolymer of vinyl chloride.According to the difference of production method, PVC can be divided into: universal polyvinyl chloride resin, PVC with high, crosslinked PVC resin.Universal polyvinyl chloride resin is polymerized under the effect of initiating agent by vinyl chloride monomer to be formed.Initiating agent is the material that energy trigger monomer carries out polyreaction, is a kind of very important product in each analog assistant of PVC, all plays an important role in each stage of PVC production link.Initiating agent directly can affect polymerization rate, also can affect the storage life of product quality, performance and product.Peroxidating two (3,5,5-trimethyl acetyl) is called for short initiating agent Tx-36 after dilution emulsification, and initiating agent Tx-36 is mixed for being polymerized of Polyvinylchloride 8 moulding mixture with initiating agent Tx-23, by the thermoplastic resin of vinyl chloride monomer under initiating agent effect.The method being detected the content of bis oxide (3,5,5-trimethyl acetyl) is at present: take 0.8g sample, be accurate to 0.0002g, be placed in iodine flask, adds 30mL glacial acetic acid tetrahydrofuran mixed solution, shake sample dissolution.Add 2.5mL liquor kalii iodide again cover bottle stopper and shake up, at 25 ± 5 DEG C, place at least 30min in dark place, be titrated to sodium thiosulfate standard solution colourless, do blank test simultaneously.The computing formula of two (3,5, the 5-trimethyl acetyl) content of peroxidating is: W={(V1-V2) × C × 0.1573}/m, wherein, in formula, and V
1
for peroxidating two (3,5,5-trimethyl acetyl) consume the numerical value of sodium thiosulfate standard titration solution volume, unit is ml, V
2
for blank test consumes the numerical value of sodium thiosulfate standard titration solution volume, unit is ml, C is the exact value of sodium thiosulfate standard titration solution concentration, unit is mol/L, m is the quality of sample, unit is g, but in the method, the reagent tetrahydrofuran used is heterocycle organic compound, it is one of strong polarity ethers, a kind of solvent of middle polarity is used as when chemical reaction and extraction, colourless volatile liquid, there is the smell of similar ether, dizziness can be there is after the tetrahydrofuran suction of high concentration, headache, uncomfortable in chest, pectoralgia, cough, weak, stomachache, dry, feel sick, the symptoms such as vomiting, can with Eye irritation symptom, Long Term Contact can cause losing sexual function, fecundity or kidney diaseases.
Summary of the invention
the invention provides peroxidating two (3 in a kind of initiating agent Tx-36,5,5-trimethyl acetyl) detection method of content, overcome the deficiency of above-mentioned prior art, it effectively can solve and detect peroxidating two (3 in initiating agent Tx-36 at present, 5,5-trimethyl acetyl) content method in the tetrahydrofuran that the uses problem large to harm.
technical scheme of the present invention is realized by following measures: peroxidating two (3 in a kind of initiating agent Tx-36, 5, 5-trimethyl acetyl) detection method of content, it carries out in the steps below: first in iodine flask, add 40mL isopropyl alcohol, 15mL glacial acetic acid and 0.5mL liquor ferri trichloridi, mix, then in iodine flask, 2min on nitrogen to liquid is led to, nitrogen flow is regulated to make liquid surface form little groove, take 0.7 to 0.9g initiating agent Tx-36 again, and after being accurate to radix point four, be placed in iodine flask, add 5mL liquor kalii iodide and cover bottle stopper, water seal immediately also shakes up, at least 30min is placed in dark place at environment temperature is 20 DEG C to 30 DEG C, add 50mL water, finally be titrated to colourless with sodium thiosulfate standard solution, meanwhile, do one group of blank test.
here is the further optimization and/or improvements to foregoing invention technical scheme:
the step of above-mentioned blank test is as follows: first in iodine flask, add 40mL isopropyl alcohol, 15mL glacial acetic acid and 0.5mL liquor ferri trichloridi, mix, then in iodine flask, 2min on nitrogen to liquid is led to, nitrogen flow is regulated to make liquid surface form little groove, add 5mL liquor kalii iodide again and cover bottle stopper, water seal immediately also shakes up, at environment temperature is 20 DEG C to 30 DEG C, place at least 30min in dark place, add 50mL water, be finally titrated to sodium thiosulfate standard solution colourless.
it is pure that above-mentioned isopropyl alcohol, glacial acetic acid are analysis, the concentration of liquor ferri trichloridi is 1g/L, nitrogen is high-purity, the concentration of liquor kalii iodide is 770g/L, iodine flask is 250mL iodine flask, the buret of titration sodium thiosulfate standard solution is brown buret, and this brown buret is 50mL buret, scale division value is 0.1mL.
in above-mentioned initiating agent Tx-36, the computing formula of two (3,5, the 5-trimethyl acetyl) content of peroxidating is: W={(V
1
-V
2
) × C × 0.1573}/m, wherein, V
1
for initiating agent Tx-36 consume the numerical value of sodium thiosulfate standard titration solution volume, unit is ml, V
2
for blank test consume the numerical value of sodium thiosulfate standard titration solution volume, the quality of unit to be ml, C be exact value that Concentration of Sodium Thiohsulfate Standard Solution demarcates, unit to be mol/L, m be sample, unit be g.
employ isopropyl alcohol in the inventive method and instead of poisonous tetrahydrofuran, decrease the harm to experimenter, and the liquor ferri trichloridi used is catalyzer, substantially reduces detection time, for testing brings great convenience, therefore, the inventive method is adopted to measure peroxidating two (3,5 in initiating agent Tx-36,5-trimethyl acetyl) content results more accurate, easy to operate, and low toxicity, be a kind of desirable detection method.
Embodiment
the present invention by the restriction of following embodiment, can not determine concrete embodiment according to technical scheme of the present invention and actual conditions.Unless stated otherwise, the % in the present invention is mass percent; Unless stated otherwise, preparation process is carried out under normal temperature, atmospheric pressure state; Unless stated otherwise, the reagent adopted in the present invention, method and apparatus are the art conventional reagent, method and apparatus; Unless stated otherwise, in the present invention, agents useful for same is commercial; Unless stated otherwise, the water in the present invention is pure water; Unless stated otherwise, the solution in the present invention is the aqueous solution that solvent is water, and such as, if illustrate, hydrochloric acid solution is aqueous hydrochloric acid solution, and preparation and the demarcation of sodium thiosulfate standard solution are carried out according to GB GB/T5009.1-2003.
below in conjunction with embodiment, the invention will be further described:
embodiment 1, peroxidating two (3 in this initiating agent Tx-36, 5, 5-trimethyl acetyl) detection method of content carries out in the steps below: first in iodine flask, add 40mL isopropyl alcohol, 15mL glacial acetic acid and 0.5mL liquor ferri trichloridi, mix, then in iodine flask, 2min on nitrogen to liquid is led to, nitrogen flow is regulated to make liquid surface form little groove, take 0.7 to 0.9g initiating agent Tx-36 again, and after being accurate to radix point four, be placed in iodine flask, add 5mL liquor kalii iodide and cover bottle stopper, water seal immediately also shakes up, at least 30min is placed in dark place at environment temperature is 20 DEG C to 30 DEG C, add 50mL water, finally be titrated to colourless with sodium thiosulfate standard solution, meanwhile, do one group of blank test.
embodiment 2, preferred as above-described embodiment, the step of blank test is as follows: first in iodine flask, add 40mL isopropyl alcohol, 15mL glacial acetic acid and 0.5mL liquor ferri trichloridi, mix, then in iodine flask, 2min on nitrogen to liquid is led to, nitrogen flow is regulated to make liquid surface form little groove, add 5mL liquor kalii iodide again and cover bottle stopper, water seal immediately also shakes up, at least 30min is placed in dark place at environment temperature is 20 DEG C to 30 DEG C, add 50mL water, be finally titrated to sodium thiosulfate standard solution colourless.
embodiment 3, preferred as above-described embodiment, it is pure that isopropyl alcohol, glacial acetic acid are analysis, the concentration of liquor ferri trichloridi is 1g/L, nitrogen is high-purity, and the concentration of liquor kalii iodide is 770g/L, and iodine flask is 250mL iodine flask, the buret of titration sodium thiosulfate standard solution is brown buret, and this brown buret is 50mL buret, scale division value is 0.1mL.
embodiment 4, preferred as above-described embodiment, in initiating agent Tx-36, the computing formula of two (3,5, the 5-trimethyl acetyl) content of peroxidating is: W={(V
1
-V
2
) × C × 0.1573}/m, wherein, V
1
for initiating agent Tx-36 consume the numerical value of sodium thiosulfate standard titration solution volume, unit is ml, V
2
for blank test consume the numerical value of sodium thiosulfate standard titration solution volume, the quality of unit to be ml, C be exact value that Concentration of Sodium Thiohsulfate Standard Solution demarcates, unit to be mol/L, m be sample, unit be g.
to contrast according to former method with according to the accuracy that the inventive method carries out two (3,5, the 5-trimethyl acetyl) content of peroxidating in detection initiating agent Tx-36:
one, adopting former method for taking 0.7g to 0.9 initiating agent Tx-36, to be accurate to after radix point four, to be placed in iodine flask, to add 30mL glacial acetic acid tetrahydrofuran mixed solution, shake sample dissolution.Add 2.5mL liquor kalii iodide again cover bottle stopper and shake up, at 20 DEG C to 30 DEG C, place at least 30min in dark place, be titrated to sodium thiosulfate standard solution colourless.Do blank test simultaneously.
formula is: W={(V
1
-V
2
) × C × 0.1573}/m.
the experimental data of former method:
it is 0.2ml that blank test consumes sodium thiosulfate standard solution, and the demarcation concentration of sodium thiosulfate standard solution is 0.1036mol/L.
test 1 group: weigh initiating agent Tx-36:0.7878g
sodium thiosulfate standard solution titration 24.6ml, substitutes into formula and obtains W1=50.47%
test 2 groups: weigh initiating agent Tx-36:0.7981g
sodium thiosulfate standard solution titration 24.5ml, substitutes into formula and obtains W2=49.62%
test 3 groups: weigh initiating agent Tx-36:0.8002g
sodium thiosulfate standard solution titration 25.3ml, substitutes into formula and obtains W3=51.12%
test 4 groups: weigh initiating agent Tx-36:0.7000g
sodium thiosulfate standard solution titration 22.2ml, substitutes into formula and obtains W3=51.22%
test 5 groups: weigh initiating agent Tx-36:0.9000g
sodium thiosulfate standard solution titration 28.2ml, substitutes into formula and obtains W3=50.70%
the variance that can obtain former method according to above data is S
2
former
=0.3276
two, the inventive method is adopted: in iodine flask, add 40mL isopropyl alcohol, 15mL glacial acetic acid and 0.5mL liquor ferri trichloridi, mix, 2min on logical nitrogen to liquid, flow of adjusting makes liquid surface form little groove, take 0.7g to 0.9g initiating agent Tx-36, to be accurate to after radix point four, be placed in iodine flask, add 5mL liquor kalii iodide and cover bottle stopper, vertical water seal also shakes up, at 20 DEG C to 30 DEG C, place at least 30min in dark place, add 50mL water, be titrated to sodium thiosulfate standard solution colourless.Do blank test simultaneously.
formula is: W={(V
1
-V
2
) × C × 0.1573}/m.
the inventive method experimental data:
it is 0.1ml that blank test consumes sodium thiosulfate standard solution, and the demarcation concentration of sodium thiosulfate standard solution is 0.1036mol/L.
test 1 group: weigh initiating agent Tx-36:0.7721g
sodium thiosulfate standard solution titration 23.8ml, substitutes into formula and obtains W1=50.02%
test 2 groups: weigh initiating agent Tx-36:0.7883g
sodium thiosulfate standard solution titration 24.3ml, substitutes into formula and obtains W2=50.23%
test 3 groups: weigh initiating agent Tx-36:0.8915g
sodium thiosulfate standard solution titration 27.6ml, substitutes into formula and obtains W3=50.45%
test 4 groups: weigh initiating agent Tx-36:0.8221g
sodium thiosulfate standard solution titration 25.4ml, substitutes into formula and obtains W4=50.15%
test 5 groups: weigh initiating agent Tx-36:0.7603g
sodium thiosulfate standard solution titration 23.4ml, substitutes into formula and obtains W5=49.94%
test 6 groups: weigh initiating agent Tx-36:0.7000g
sodium thiosulfate standard solution titration 21.7ml, substitutes into formula and obtains W6=50.29%
test 7 groups: weigh initiating agent Tx-36:0.9000g
sodium thiosulfate standard solution titration 27.8ml, substitutes into formula and obtains W7=50.16%
the variance S of the inventive method can be obtained according to above data
2
send out
=0.0249
by S
2
newly
< S
2
send out
known, adopt the content of peroxidating two (3,5,5-trimethyl acetyl) in the inventive method mensuration initiating agent Tx-36 more accurate than former method.
employ isopropyl alcohol in the inventive method and instead of poisonous tetrahydrofuran, decrease the harm to experimenter, and the liquor ferri trichloridi used is catalyzer, substantially reduces detection time, for testing brings great convenience, therefore, the inventive method is adopted to measure peroxidating two (3,5 in initiating agent Tx-36,5-trimethyl acetyl) content results more accurate, easy to operate, and low toxicity, be a kind of desirable detection method.
above technical characteristic constitutes embodiments of the invention, and it has stronger adaptability and implementation result, can increase and decrease non-essential technical characteristic according to actual needs, meet the demand of different situations.
Claims (5)
1. peroxidating two (3 in an initiating agent Tx-36, 5, 5-trimethyl acetyl) detection method of content, it is characterized in that carrying out in the steps below: first in iodine flask, add 40mL isopropyl alcohol, 15mL glacial acetic acid and 0.5mL liquor ferri trichloridi, mix, then in iodine flask, 2min on nitrogen to liquid is led to, nitrogen flow is regulated to make liquid surface form little groove, take 0.7 to 0.9g initiating agent Tx-36 again, and after being accurate to radix point four, be placed in iodine flask, add 5mL liquor kalii iodide and cover bottle stopper, water seal immediately also shakes up, at least 30min is placed in dark place at environment temperature is 20 DEG C to 30 DEG C, add 50mL water, finally be titrated to colourless with sodium thiosulfate standard solution, meanwhile, do one group of blank test.
2. peroxidating two (3 in initiating agent Tx-36 according to claim 1, 5, 5-trimethyl acetyl) detection method of content, it is characterized in that the step of blank test is as follows: first in iodine flask, add 40mL isopropyl alcohol, 15mL glacial acetic acid and 0.5mL liquor ferri trichloridi, mix, then in iodine flask, 2min on nitrogen to liquid is led to, nitrogen flow is regulated to make liquid surface form little groove, add 5mL liquor kalii iodide again and cover bottle stopper, water seal immediately also shakes up, at least 30min is placed in dark place at environment temperature is 20 DEG C to 30 DEG C, add 50mL water, finally be titrated to colourless with sodium thiosulfate standard solution.
3. peroxidating two (3 in initiating agent Tx-36 according to claim 1 and 2,5,5-trimethyl acetyl) detection method of content, it is characterized in that isopropyl alcohol, glacial acetic acid be analyze pure, the concentration of liquor ferri trichloridi is 1g/L, and nitrogen is high-purity, the concentration of liquor kalii iodide is 770g/L, iodine flask is 250mL iodine flask, and the buret of titration sodium thiosulfate standard solution is brown buret, and this brown buret is 50mL buret, scale division value is 0.1mL.
4. two (3,5,5-trimethyl acetyl) detection method of content of peroxidating in initiating agent Tx-36 according to claim 1 and 2, is characterized in that the computing formula of two (3,5,5-trimethyl acetyl) content of peroxidating in initiating agent Tx-36 is: W={(V
1-V
2) × C × 0.1573}/m, wherein, V
1for initiating agent Tx-36 consume the numerical value of sodium thiosulfate standard titration solution volume, unit is ml, V
2for blank test consume the numerical value of sodium thiosulfate standard titration solution volume, the quality of unit to be ml, C be exact value that Concentration of Sodium Thiohsulfate Standard Solution demarcates, unit to be mol/L, m be sample, unit be g.
5. two (3,5,5-trimethyl acetyl) detection method of content of peroxidating in initiating agent Tx-36 according to claim 3, is characterized in that the computing formula of two (3,5,5-trimethyl acetyl) content of peroxidating in initiating agent Tx-36 is: W={(V
1-V
2) × C × 0.1573}/m, wherein, V
1for initiating agent Tx-36 consume the numerical value of sodium thiosulfate standard titration solution volume, unit is ml, V
2for blank test consume the numerical value of sodium thiosulfate standard titration solution volume, the quality of unit to be ml, C be exact value that Concentration of Sodium Thiohsulfate Standard Solution demarcates, unit to be mol/L, m be sample, unit be g.
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