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Method for measuring monomer conversion rate in additive synthetic process

A technology of monomer conversion rate and synthesis process, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of long measurement time, inability to achieve rapid measurement, etc., and achieve the effect of short detection time, fewer samples, and simple process.

Active Publication Date: 2015-12-30
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of long measurement time and inability to realize rapid measurement when the existing method is used to measure the monomer conversion rate in the additive synthesis process, and to provide a method that can quickly and accurately measure the additive Method for monomer conversion during synthesis

Method used

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  • Method for measuring monomer conversion rate in additive synthetic process
  • Method for measuring monomer conversion rate in additive synthetic process
  • Method for measuring monomer conversion rate in additive synthetic process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: establish the standard concentration of polybutylmethacrylate and the linear function relational expression of peak area

[0035] (1) Establish a linear function relational expression:

[0036] Dissolve 5 g of polybutyl methacrylate (produced by Polymer Standers Service GmbH, with a number-average molecular mass of 105,000) in 200 mL of tetrahydrofuran, transfer the resulting solution to a 500 mL volumetric flask, dilute to volume with tetrahydrofuran, shake well, and prepare a polymer Butyl methacrylate mass concentration is the standard solution of 10g / L. Then this solution is diluted to the polybutylmethacrylate standard solution of 0.5g / L, 1.0g / L, 1.5g / L, 2.0g / L and 4.0g / L respectively, and carries out gel permeation chromatography analysis respectively, A unique peak appears on the gel chromatogram, and the time interval from appearance to disappearance of the peak is 15.90-16.10 min, and the peak area integrated by the chromatographic workstation is...

Embodiment 2

[0041] Example 2: Determination of monomer conversion rate when polymethacrylate type pour point depressant A is synthesized for 3 hours

[0042] Under the protection of nitrogen, add 20g base oil (purchased from Ssangyong Company, the brand is 100N, the same below) in the reactor equipped with mechanical stirring, then add 80g methacrylate (decyl methacrylate, methacrylic acid Lauryl ester and stearyl methacrylate are a mixture of 1:1:1 by weight, the same below), an appropriate amount of benzoyl peroxide and dodecyl mercaptan are mixed into the above-mentioned reaction kettle, and then The reaction kettle was heated to 91-103°C, stirred rapidly and the reaction temperature was maintained at 91-103°C. After reacting for 3 hours, weigh 0.6 g of the reaction material and dissolve it in 200 mL of tetrahydrofuran, and transfer the obtained solution to a 500 mL volumetric flask, dilute to volume with tetrahydrofuran, shake well, and prepare a concentration of 1.2 g / L (polymethacry...

Embodiment 3

[0043] Example 3: Measurement of monomer conversion rate when polymethacrylate type pour point depressant A was synthesized for 5 hours

[0044] The synthesis process of polymethacrylate type pour point depressant A is the same as in Example 2.

[0045] After reacting for 5 hours, weigh 0.7 g of the reaction material and dissolve it in 200 mL of tetrahydrofuran, and transfer the resulting solution to a 500 mL volumetric flask, dilute to volume with tetrahydrofuran, shake well, and prepare a concentration of 1.4 g / L (polymethacrylate The theoretical concentration is 1.12g / L) standard solution. Then this solution is carried out gel permeation chromatography analysis under the chromatographic operating condition identical with embodiment 1, two spectral peaks appear on the gel chromatogram, the spectral peak of polymethacrylate is from the time interval of appearance to disappearance For 13.90-18.70min, record the peak area integrated by the chromatographic workstation. The sam...

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Abstract

The invention provides a method for measuring the monomer conversion rate in the additive synthetic process. The method includes the steps of firstly, establishing the linear function relational expression between the normal concentration of effective components or effective component analog in to-be-measured additives and the peak area, obtained according to the gel permeation chromatography, of the effective components or the effective component analog; secondly, conducting gel permeation chromatography on a solution of the to-be-measured additives to obtain the peak area of the effective components in the solution of the to-be-measured additives, substituting the peak area into the linear function relational expression in the first step, calculating the concentration of the effective components, and determining the monomer conversion rate according to the ratio of the concentration of the effective components to the theoretical concentration. When the monomer conversion rate in the additive synthetic process is measured through the method, the whole process is quite simple, the number of required samples is small, the synthetic reaction of the additives is not influenced after sampling, the detection time is short, measured data are accurate, the monomer conversion degree in the additive synthetic process can be truly reflected, and extremely good industrial application prospects are achieved.

Description

technical field [0001] The invention relates to a method for measuring monomer conversion rate in additive synthesis process. Background technique [0002] Monomer conversion rate is one of the most important indicators reflecting the synthesis process of additives. During the synthesis of many oil additives, 1%-99% diluent oil needs to be added. On the one hand, the addition of diluent oil can improve the problems of mass transfer and heat transfer caused by high viscosity in the additive synthesis process, and on the other hand, it can also provide a stable dispersion place for the active components in the additive, and effectively relieve the additive Inconvenience to the transportation and adding process due to high viscosity. Typically, diluent oils are distillate oils, low viscosity white oils and lube base oils. In industrial production, after the synthesis or processing of the additive, the diluent oil and the effective component of the additive are no longer sepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 张耀段庆华刘依农李玲辛世豪
Owner CHINA PETROLEUM & CHEM CORP
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