A kind of assay method of p-toluenesulfonic acid content in butyl acrylate reactor
A technology of p-toluenesulfonic acid and butyl acrylate, which is used in chemical analysis, measuring devices, instruments and other directions by titration, which can solve problems such as inaccurate results and impact on production control.
Active Publication Date: 2016-06-22
谦信化工集团有限公司 +1
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Problems solved by technology
However, the content of acrylic acid is so high that the results obtained by titration alone are inaccurate and affect the production control
Method used
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Experimental program
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Effect test
Embodiment 1
[0015] The assay method of p-toluenesulfonic acid content in a kind of butyl acrylate reactor described in present embodiment 1, the specific of this assay method is: add 50ml dehydrated alcohol and 2-3 drop 0.1g / L in 250ml conical flask Phenolphthalein, titrate to reddish with 0.1mol / L sodium hydroxide standard solution, ignore the reading, add sample mass m=2-3g (accurate sample weight) into the conical flask, use C=0.1mol / L sodium hydroxide standard The solution is titrated to a reddish color, and the end point is reached without fading within 30s, and the volume V of sodium hydroxide consumed is recorded.
[0016] Draw 1ml of sample into the chromatographic bottle, then put it into the autosampler, call the detection method of acrylic acid, run it after confirmation, read the mass percentage X1 of acrylic acid after the method is run, and calculate the hydrogen consumption of acrylic acid according to the calculation formula of acrylic acid Sodium volume V1.
[0017] Draw...
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The invention discloses a method for determining content of p-toluenesulfonic acid in a butyl acrylate reaction kettle. The method for determining the content of p-toluenesulfonic acid in the butyl acrylate reaction kettle comprises the following steps: adding absolute alcohol and a phenolphthalein indicator into a triangular flask, titrating to be reddish with a sodium hydroxide solution, accurately weighing a certain quantity of samples into the triangular flask, titrating to be reddish with a sodium hydroxide standard solution, and recording volume consumed at the moment; correcting acrylic acid by virtue of an external standard method by adopting an automatic sampling gas chromatograph, accurately determining mass percentage of acrylic acid in the samples, and carrying out reverse calculation to obtain volume of sodium hydroxide consumed by acrylic acid according to an acrylic acid calculation formula; subtracting to obtain volume of sodium hydroxide consumed by p-toluenesulfonic acid, and obtaining mass percentage of p-toluenesulfonic acid according to a p-toluenesulfonic acid calculation formula. The method disclosed by the invention has the advantages that the content of p-toluenesulfonic acid in the butyl acrylate reaction kettle can be accurately determined, and a great effect on stably controlling the content of a reaction kettle catalyst is realized.
Description
technical field [0001] The present invention relates to the technical field of a method for measuring in chemical production, in particular to a method for measuring p-toluenesulfonic acid content in a butyl acrylate reactor. Background technique [0002] P-toluenesulfonic acid is a non-oxidizing organic strong acid, white needle-like or powder crystal, easy to deliquescence, soluble in water, alcohol and other polar solvents, widely used as a catalyst in the production of acrylate, from the reactor Addition is started, and then it is extracted and recovered for reuse. [0003] The general determination method of p-toluenesulfonic acid is titration method: titrate with sodium hydroxide standard solution, use phenolphthalein as indicator, record the consumed volume of sodium hydroxide to calculate the content. This method is based on the fact that when there is no other acidic substance or the content of other acidic substance is low, the determination result is more accurat...
Claims
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IPC IPC(8): G01N31/16G01N30/02
Inventor 赵楚榜于冬娥李成富胡子达
Owner 谦信化工集团有限公司