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Extraction agent and method for measuring free amine content in spandex spinning stock solution

A spinning dope and extractant technology, applied in the field of spandex production process control, can solve the problems of high viscosity of spandex spinning dope, unable to meet the needs of detection, difficult to escape free amine, etc., and achieve wide applicability and good accuracy. , the extraction effect is good

Active Publication Date: 2021-06-29
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, due to the high viscosity of spandex spinning dope, generally 100-800Pa·s, the content of free amine in it is relatively low, generally less than 100ppm, which makes it difficult for free amine to escape and be detected by conventional methods
Even if a good solvent is used to dilute the spandex spinning stock solution and then perform headspace-gas chromatography, the detection recovery rate is still low, which cannot meet the detection needs

Method used

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  • Extraction agent and method for measuring free amine content in spandex spinning stock solution
  • Extraction agent and method for measuring free amine content in spandex spinning stock solution
  • Extraction agent and method for measuring free amine content in spandex spinning stock solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The mensuration of free amine in the spandex spinning dope produced by the continuous process of embodiment 1

[0031] This embodiment takes the spandex spinning dope produced by the continuous process of the spandex factory as an example. In the production process of the spandex spinning stock solution of this embodiment, the molar ratio (R value) of NCO to OH in the prepolymerization stage is 1.66, and the prepolymer is dissolved with solvent DMAc, and the solid content is 35wt%; in the chain extension stage, NH 2 The molar ratio (A / N) to NCO is 1.05, the amine chain extender is ethylenediamine and 1,2-propylenediamine, and the amine terminator is diethylamine.

[0032] The extractant used in this example is the main reagent (purchased from TCI company, 1-propionyl-2-pyrrolidone) and auxiliary reagent (purchased from Dow Chemical, Triton x-100) composition, wherein the mass percentage of auxiliary reagents is 10%.

[0033] Take 10g (accurate to 0.1mg) of spandex ...

Embodiment 2

[0042] Example 2 Determination of free amine in spandex spinning stock solution produced by batch process

[0043] In this embodiment, the spandex spinning dope produced by the batch process in a spandex factory is taken as an example. In the production process of the spandex spinning stock solution of this embodiment, the molar ratio (R value) of NCO to OH in the prepolymerization stage is 1.80, and the prepolymer is dissolved with solvent DMAc, and the solid content is 35wt%; in the chain extension stage, NH 2 The molar ratio (A / N) to NCO is 1.05, the amine chain extender is 1,2-pentanediamine, and the amine terminator is di-n-butylamine.

[0044] The extractant used in this example is the main reagent (purchased from Huaxia Chemical Reagent Co., Ltd., 1-n-pentanoyl-2-pyrrolidone) and auxiliary reagents (purchased from Beijing Huayueyang Biology, Tritonx-114), wherein the mass percentage of auxiliary reagents is 20%.

[0045] Take 10g (accurate to 0.1mg) of spandex spin...

Embodiment 3

[0054] This embodiment takes the spandex spinning dope produced by the continuous process of the spandex factory as an example. In the production process of the spandex spinning stock solution of this embodiment, the molar ratio (R value) of NCO to OH in the prepolymerization stage is 1.70, and the prepolymer is dissolved with solvent DMAc, and the solid content is 35wt%; in the chain extension stage, NH 2 The molar ratio (A / N) to NCO is 1.03, the amine chain extender is ethylenediamine, and the amine terminator is diethylamine.

[0055] The extractant used in this example is the main reagent (TCI company, 1-acetyl-2-pyrrolidone) and auxiliary reagents (Dow Chemical, Triton x-100), wherein the mass percentage of auxiliary reagents is 20%.

[0056] Take 10g (accurate to 0.1mg) of spandex spinning stock solution in a 50mL centrifuge tube, add 30g (accurate to 0.1mg) of the above extractant, seal the centrifuge tube, and mix for 5min with a shaker; at the same time, make parall...

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Abstract

The present invention provides an extractant and a method for measuring the content of free amine in spandex spinning stock solution. The extractant provided by the present invention includes a main reagent and a secondary reagent, and the main reagent includes the compound shown in the following formula (I): At least one, the secondary reagent is a compound with a hydrophilic end and a hydrophobic end in the molecular structure: wherein, R in the formula (I) is, n in R is an integer of 0-10, and n is further preferably 0-5 an integer of . Utilizing the extractant of the invention to extract the free amine in the spandex spinning dope is beneficial to accurately quantify the content of the free amine therein.

Description

technical field [0001] The invention relates to the field of spandex production process control, in particular to an extractant and a method for measuring free amine content in spandex spinning stock solution by using the extractant. Background technique [0002] In the production process of spandex, polytetrahydrofuran ether diol and diisocyanate are generally used as raw materials for mixed reaction to obtain isocyanate-terminated prepolymer, and then the prepolymer is dissolved with amide compound and mixed with amine chain extender and terminator to obtain polyurethane Urea solution (or called spandex spinning solution). Generally, in the production process, an excess of amine is used in the chain extension reaction, so in the obtained polyurethaneurea solution, there are unreacted amine chain extenders and amine terminators (ie free amines), and macromolecular chain ends. Reactive amino groups (i.e. blocked amines). In the technical field, the two amines are usually c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/00G01N30/02G01N30/06
Inventor 高振华许钦一徐丹苏昕金振宇王文博张宏科
Owner WANHUA CHEM GRP CO LTD
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