A method for measuring the conversion rate of monomer in additive synthesis process

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

Active Publication Date: 2017-12-22
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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  • A method for measuring the conversion rate of monomer in additive synthesis process
  • A method for measuring the conversion rate of monomer in additive synthesis process
  • A method for measuring the conversion rate of monomer in additive synthesis 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] 5g of polybutyl methacrylate (produced by Polymer Standers Service GmbH company, the number-average molecular mass is 105,000) was dissolved in 200mL of tetrahydrofuran, and the resulting solution was transferred to a 500mL volumetric flask, constant volume with tetrahydrofuran, shaken, Prepare a standard solution with a mass concentration of polybutyl methacrylate of 10 g / 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 works...

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 monomer conversion rate in the process of measuring additive synthesis, the method comprising: (1) establishing the standard concentration of the effective component or the analog of the effective component in the additive to be tested and analyzing according to gel permeation chromatography The linear function relational expression of the peak area of ​​this effective component or effective component analogue that obtains; (2) carry out gel permeation chromatographic analysis with the solution of additive to be tested, obtain the effective component in the solution of described additive to be tested Peak area, this peak area is substituted in the linear function relational formula described in step (1), calculates the concentration of described effective component, and determines the conversion rate of monomer according to the ratio of the concentration of this effective component and theoretical concentration . The above method is used to measure the conversion rate of monomers in the process of additive synthesis. The whole process is very simple, requires few samples, does not affect the synthesis reaction of additives after sampling, the detection time is short and the test data is accurate, which can truly reflect the monomers in the process of additive synthesis. The conversion degree of the body has great industrial application prospects.

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 Patents(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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