阅读说明：本技术 一种涤纶/锦纶6混纺产品的定量分析方法 (Quantitative analysis method of terylene/chinlon 6 blended product ) 是由 张静静 郭文娟 李王思芸 李建君 安嘉慧 王双 于 2020-04-15 设计创作，主要内容包括：本发明涉及混纺产品的定量分析领域,具体涉及一种涤纶/锦纶6混纺产品的定量分析方法,所述混纺产品由涤纶和锦纶6组成,采用差示扫描量热分析仪对所述涤纶/锦纶6混纺产品进行扫描,具体为：将测试样品剪碎、装入坩埚、称重,升温至280℃,试样中两组分熔融,维持一段时间,消除热历史,然后由280℃降温至30℃,试样中两组分结晶；再次升温至280℃,用差示扫描量热分析仪对所述涤纶/锦纶6混纺产品进行扫描,得到ΔH-(测试样品-涤纶)和ΔH-(测试样品-锦纶6)；利用式(I)、式(II)计算测试样品的组分含量：(The invention relates to the field of quantitative analysis of blended products, in particular to a quantitative analysis method of a terylene/chinlon 6 blended product, wherein the blended product consists of terylene and chinlon 6, a differential scanning calorimetry analyzer is adopted to scan the terylene/chinlon 6 blended product, and the method specifically comprises the following steps: cutting a test sample, putting the test sample into a crucible, weighing, heating to 280 ℃, melting two components in the test sample, maintaining for a period of time, eliminating thermal history, and then cooling from 280 ℃ to 30 ℃, and crystallizing the two components in the test sample; raising the temperature to 280 ℃ again, and scanning the terylene/chinlon 6 blended product by using a differential scanning calorimetry analyzer to obtain delta H Test sample-polyester And Δ H Test sample-Jinlun 6 (ii) a Calculating the component content of the test sample by using the formula (I) and the formula (II):)

1. A quantitative analysis method for a terylene/chinlon 6 blended product is characterized in that the blended product consists of terylene and chinlon 6, a differential scanning calorimetry analyzer is adopted to scan the terylene/chinlon 6 blended product, and the method comprises the following steps:

(1) shearing a test sample, putting the test sample into a crucible, and weighing the mass of the test sample;

(2) heating to 280 ℃, melting the two components, and maintaining for a period of time to eliminate thermal history;

(3) cooling from 280 ℃ to 30 ℃, and crystallizing the two components;

(4) raising the temperature to 280 ℃ again, crystallizing and melting the two components, and scanning the terylene/chinlon 6 blended product by using a differential scanning calorimetry analyzer to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}；

(5) Calculating the component content of the test sample by using the formula (I) and the formula (II):

wherein Δ H_{Test sample-polyester}Is the melting enthalpy value, delta H, of the terylene component in the terylene/chinlon 6 blended product_TeryleneThe enthalpy value of the fusion of the polyester raw material under the same thermal history condition; Δ H_{Test sample-Jinlun 6}Is the melting enthalpy value, delta H, of the chinlon 6 component in the terylene/chinlon 6 blended product_Nylon-6Is the melting enthalpy value of the chinlon 6 raw material under the same thermal history condition.

2. The quantitative analysis method of the terylene/chinlon 6 blended product according to claim 1, wherein in the step (1), the sample is cut into 30-100 meshes.

3. The quantitative analysis method of the terylene/chinlon 6 blended product according to claim 1, wherein in the step (2), the maintaining time is 1-8 minutes, preferably 3-5 minutes.

4. The quantitative analysis method of the terylene/chinlon 6 blended product according to claim 1, wherein in the step (3), the cooling rate is 0.1-5 ℃/min.

5. The quantitative analysis method of the terylene/chinlon 6 blended product according to claim 1, wherein in the step (4), the temperature rise rate is 5 ℃/min to 20 ℃/min.

6. The quantitative analysis method of the terylene/chinlon 6 blended product according to claim 1, characterized in that the determination method of the melting enthalpy of the terylene and chinlon 6 raw materials is the same as the determination method of the terylene/chinlon 6 blended product.

7. The quantitative analysis method of the terylene/chinlon 6 blended product according to claim 1, wherein the terylene and the chinlon 6 in the blended product are both in mass percent: w% is more than or equal to 0 and less than or equal to 100.

Technical Field

The invention relates to the field of quantitative analysis of blended products, in particular to a quantitative analysis method of a terylene/chinlon 6 blended product.

Background

With the development of society and the improvement of living standard of people, the application of the terylene/chinlon 6 blended product in the clothing textile and the home textile is more and more. The terylene has excellent acid and alkali resistance, the chinlon 6 has better wear resistance and moisture absorption, and the blended product of the terylene and the chinlon has the characteristics of moisture absorption, ventilation, lightness, thinness, softness, durability and the like, so the blended product has wider and wider application range in daily textiles.

However, the prices of terylene and chinlon 6 in international markets are different, and the product price and the use effect are different. In the current stage, a dissolution method and a manual decomposition method are mainly adopted for quantitative analysis of the terylene/chinlon 6 blended product, but for terylene and chinlon 6, on one hand, the terylene/chinlon 6 blended product has less soluble solvents, mostly strong polar solvents and higher toxicity; on the other hand, the solvent method inevitably produces a large amount of waste liquid, which causes environmental pollution, and environmental and artificial factors have certain influence on the result. The manual decomposition method is time-consuming and labor-consuming, and some products cannot be decomposed manually. Therefore, research and development of accurate, reliable and simple quantitative analysis methods for terylene/chinlon 6 blended products are urgent.

Differential scanning calorimetry is a method for measuring thermodynamic and kinetic parameters of a sample, such as transformation heat, crystallization rate, crystallinity of high polymer, purity of the sample and the like, at a program controlled temperature, and has the advantages of wide application range, high resolution, good accuracy and the like. Through a large number of touch cord tests and researches, the melting temperature difference of the terylene and the chinlon 6 is about 30 ℃, the melting of the two components is not influenced mutually, and necessary conditions are provided for realizing the invention.

Disclosure of Invention

The invention aims to provide a quantitative analysis method for a terylene/chinlon 6 blended product.

In order to realize the purpose of the invention, the technical scheme is as follows:

a quantitative analysis method for a terylene/chinlon 6 blended product, the blended product consists of terylene and chinlon 6, a differential scanning calorimetry analyzer is adopted to scan the blended product, and the specific method comprises the following steps:

(1) shearing a test sample, putting the test sample into a crucible, and weighing the mass of the test sample; the accurate weighing of the sample is to ensure the accuracy of the test data, and the quality of the sample is controlled to be 5-10 mg;

(2) heating to 280 ℃, melting the two components, and maintaining for a period of time to eliminate thermal history;

(3) cooling from 280 ℃ to 30 ℃, and crystallizing the two components;

(4) raising the temperature to 280 ℃ again, crystallizing and completely melting the two components, and scanning the terylene/chinlon 6 blended product by using a differential scanning calorimetry analyzer to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}；

(5) Calculating the component content of the test sample by using the formula (I) and the formula (II):

wherein Δ H_{Test sample-polyester}Is the melting enthalpy value, delta H, of the terylene component in the terylene/chinlon 6 blended product_TeryleneThe enthalpy value of the fusion of the polyester raw material under the same thermal history condition; Δ H_{Test sample-Jinlun 6}Is the melting enthalpy value, delta H, of the chinlon 6 component in the terylene/chinlon 6 blended product_Nylon-6Is the melting enthalpy value of the chinlon 6 raw material under the same thermal history condition.

The first preferred technical scheme of the invention is as follows: in the step (1), the sample is cut into 30-100 meshes.

The second preferred technical scheme of the invention is as follows: in the step (2), the maintaining time is 1 to 8 minutes, preferably 3 to 5 minutes.

The third preferred technical scheme of the invention is as follows: in the step (3), the cooling rate is 0.1-5 ℃/min.

The fourth preferred technical scheme of the invention is as follows: in the step (4), the heating rate is 5-20 ℃/min.

The fifth preferred technical scheme of the invention is as follows: the determination method of the melting enthalpy value of the terylene and the chinlon 6 raw materials is the same as the determination method of the terylene/chinlon 6 blended product.

The sixth preferred technical scheme of the invention is as follows: the blended product comprises the following components in percentage by mass: w% is more than or equal to 0 and less than or equal to 100.

The technical solution of the present invention is further explained and illustrated below.

Aiming at the defects of the prior art, the invention provides the quantitative analysis method of the terylene/chinlon 6 blended product, which is accurate, reliable, simple and convenient to operate, energy-saving and environment-friendly. And scanning the terylene/chinlon 6 blended product by using a differential scanning calorimetry analyzer according to the property difference between the melting temperatures of terylene and chinlon 6 in the blended product, and calculating to determine the content of each component.

Wherein, in step 1, the sample is clipped to reduce hysteresis during scanning;

in the step 2, the temperature is raised to 280 ℃, the terylene and the chinlon 6 are melted, and the constant temperature is kept for a period of time so as to ensure that the thermal history of the terylene and the chinlon 6 is completely eliminated;

in the step 3, the cooling speed needs to be controlled to ensure that the terylene and the chinlon 6 are completely crystallized;

in step 4, the rate of re-heating needs to be controlled, because if the rate of heating is too slow, the response of the instrument signal is weak; if the temperature rise rate is too fast, the fusion enthalpy values of the terylene and the chinlon 6 are influenced in a cross way, so that the accuracy of data is influenced.

The invention has the beneficial effects that: compared with the traditional fiber quantitative analysis method, the method disclosed by the invention has the advantages that the quantitative analysis is carried out on the terylene/chinlon 6 blended product, no chemical reagent is used, the energy is saved, the environment is protected, meanwhile, the method is simple to operate, the influence of environmental and human factors is effectively reduced, the result is accurate and reliable, and the reproducibility is good.

The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the present invention, but rather as providing those skilled in the art with the necessary modifications and adaptations to the present invention in light of the above teachings.

Detailed Description

Example 1

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) 40: 60, cutting the terylene/chinlon 6 blended product into 60 meshes, putting into a crucible, and accurately weighing the mixture to 7.15 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 4min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at 1.5 ℃/min; heating to 280 ℃ at the speed of 8 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 41: 59.

Example 2

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) of the polyester/chinlon 6 blended product is cut into 45 meshes, and the mixture is put into a crucible, and the mass of the mixture is accurately weighed to be 5.00 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 1min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at the speed of 0.1 ℃/min; heating to 280 ℃ at a speed of 10 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 80: 20.

Example 3

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) is 50: 50, the terylene/chinlon 6 blended product is cut into 30 meshes and is put into a crucible, and the weight of the terylene/chinlon 6 blended product is accurately weighed to be 5.96 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 4min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at the speed of 2 ℃/min; at 14 deg.CHeating to 280 deg.C/min, and detecting to obtain Δ H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 49: 51.

Example 4

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) of the polyester/chinlon 6 blended product is cut into 70 meshes, and the mixture is put into a crucible, and the mass of the mixture is accurately weighed to be 6.32 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 3min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at a speed of 4 ℃/min; heating to 280 ℃ at a speed of 20 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 100: 0.

Example 5

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) of the polyester/chinlon 6 blended product is cut into 80 meshes, and the mixture is put into a crucible, and the mass of the mixture is accurately weighed to be 7.28 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 5min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at a speed of 1 ℃/min; heating to 280 ℃ at the speed of 6 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 18: 82.

Example 6

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) 30: 70, cutting the terylene/chinlon 6 blended product into 40 meshes, putting into a crucible, and accurately weighing the terylene/chinlon 6 blended product with the mass of 8.20 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 8min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at the speed of 0.5 ℃/min; heating to 280 ℃ at the speed of 12 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 30: 70.

Example 7

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) is 0: 100, the terylene/chinlon 6 blended product is cut into 90 meshes and is put into a crucible, and the weight of the terylene/chinlon 6 blended product is accurately weighed to be 10.00 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 7min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at 3 ℃/min; heating to 280 ℃ at a speed of 15 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 0: 100.

Example 8

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) is 66: 34, the terylene/chinlon 6 blended product is cut into pieces of 100 meshes and is put into a crucible, and the weight of the mixture is accurately weighed to be 8.36 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 2min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at the speed of 2.5 ℃/min; heating to 280 ℃ at the speed of 5 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-brocadeNylon 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 65: 35.

Example 9

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) of the polyester/chinlon 6 blended product is cut into 35 meshes, and the mixture is put into a crucible, and the mass of the mixture is accurately weighed to be 9.31 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 6min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at a speed of 5 ℃/min; heating to 280 ℃ at the speed of 18 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 68: 32.

Example 10

The mass composition ratio (w)_Terylene％∶w_Nylon-6%) is 10: 90, the terylene/chinlon 6 blended product is cut into 50 meshes and is put into a crucible, and the weight of the terylene/chinlon 6 blended product is accurately weighed to be 6.78 mg; heating to 280 ℃, completely melting the terylene and the chinlon 6, keeping for 5min, and scanning the blended product by using a differential scanning calorimetry analyzer; then reducing the temperature to 30 ℃ at 3.5 ℃/min; heating to 280 ℃ at the speed of 16 ℃/min, and detecting to obtain delta H_{Test sample-polyester}And Δ H_{Test sample-Jinlun 6}And measuring the melting enthalpy value delta H of the terylene and the chinlon 6 raw materials under the same thermal history condition_TeryleneΔH_Nylon-6(ii) a Calculating the content of the terylene and the chinlon 6 according to the formula (I) and the formula (II) to obtain the mass composition ratio (w) of the terylene to the chinlon 6_Terylene％∶w_Nylon-6%) was 11: 89.