CN101598722B - Oxidizing digestion method for polyamide fiber - Google Patents
Oxidizing digestion method for polyamide fiber Download PDFInfo
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- CN101598722B CN101598722B CN 200910054388 CN200910054388A CN101598722B CN 101598722 B CN101598722 B CN 101598722B CN 200910054388 CN200910054388 CN 200910054388 CN 200910054388 A CN200910054388 A CN 200910054388A CN 101598722 B CN101598722 B CN 101598722B
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Abstract
The invention relates to an oxidizing digestion method for polyamide fiber, comprising the following steps: putting potassium dichromate solution, water, zeolite and a polyamide fiber sample in cold bath; slowly adding mixture of silver sulfate and sulphuric acid to a container while stirred at low speed; connecting a ball condenser pipe to the container and communicating with fluid condensate water; heating digestion solution in a bottle until the digestion solution is boiled; pouring the digestion solution to a clean glass beaker after the digestion ends; then cleaning the bottle; collecting cleaning solution and mixing the cleaning solution with the digestion solution; putting the glass beaker in the cold bath, and slowly adding alkaline substances to make the digestion solution to be neutral. The invention ensures that the polyamide fiber is completely oxidized and digested into simple compounds, and the detectable quantity of carbon element and nitrogen element is lower than 0.05% after digestion products are tested by an element analyzer. Thus, the invention is suitable for sample digestion treatment before micro-substance in textile is detected.
Description
Technical field
The invention belongs to the textile fibres oxidation and clear up technical field, particularly relate to a kind of oxidizing digestion method of polyamide fibre.
Background technology
Continuous enhancing along with human consumption's level and environmental protection consciousness; various countries increase day by day to the test item of objectionable impurities in the textile; European Union has successively put into effect laws and regulations and the associated documents of the ecological textile aspects such as OEKOTEX STANDARD 100, REACH rules; the Chinese government has also promulgated corresponding rule and standard; yet China reaches in the world and still be at present relatively blank state on the method that relevant textile objectionable impurities detects.In the detection document of objectionable impurities, what the overwhelming majority adopted is extraction in the textile of having carried out at present, and this method operation is fairly simple, but different material need to be sought different extractants, and testing result is subject to the impact of extraction efficiency easily.For the project that detects with methods such as chromatogram, mass spectrums, the organism that exists on the fiber might bring many interference to testing result, affects the precision of testing result, even causes test item correctly to judge.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of oxidizing digestion method of polyamide fibre, by custom-designed oxidation Acid system, make polyamide fibre under certain condition exhaustive oxidation clear up and be simple compounds, avoid the interference of organic compound to testing result, provide favourable basis to the detection of microscale harmful substance in the textile.This method is applicable to the sample pre-treatments before the objectionable impurities detection in various polyamide fibres and the blended product thereof.
The invention provides a kind of oxidizing digestion method of polyamide fibre, comprise the steps:
By the chemical oxidation Acid system that potassium dichromate, silver-colored sulfate, sulfuric acid and water form, potassium dichromate is made certain density aqueous solution in advance; Silver sulfate and sulfuric acid are made a certain proportion of mixed liquor in advance;
The digestion instrument that is formed by ground conical flask or round-bottomed flask, spherical reflux condensing tube, gas burning lamp or electric furnace, asbestos gauge, iron stand; Connect flowing cool water in the shape reflux condensing tube of receiving on ground conical flask or the round-bottomed flask bottleneck, condenser pipe;
Digestion solution forms:
Polyamide fibre goods: 0.0100g～1.0000g;
Potassium bichromate solution (concentration 0.5000～1.5000mol/L): 5～100ml;
Silver sulfate/sulfuric acid mixture liquid: 15～200ml (Ag
2SO
4: H
2SO
4=1: 3 (V/V);
Distilled water: 20～150ml;
Get potassium bichromate solution, 20～150ml water, a small amount of zeolite and 0.0100～1.0000g polyamide fibre sample that 5.0～100ml concentration is 0.5000～1.5000mol/L, join successively in ground conical flask or the round-bottomed flask, said vesse is placed cooling bath, get again pre-configured silver sulfate and sulfuric acid mixture liquid (Ag
2SO
4: H
2SO
4=1: 3V/V) 15～150ml, under the condition of low rate mixing, slowly join in the container, connect spherical condensation tube and connect flow condensation water, open thermal source, digestion solution in the container is heated to boils, timing, digestion time is from the digestion solution boiling 2～3 hours, during clearing up, adjusting adds heat and keeps digestion solution to be slight boiling condition, clears up end, and digestion solution is poured onto in the clean glass beaker, with distilled water digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into.Glass beaker is placed in the cooling bath, slowly add alkaline matter and make digestion solution be neutralized to neutrality.
Described thermal source is a kind of in natural gas, artificial water gas or the electrical heating, and heating-up temperature is 125～150 ℃.
In this method, the purity of clearing up used chemicals is to be analyzed purely, and water is distilled water, used alkaline matter is solid-state or aqueous potassium hydroxide, NaOH in a kind of.
The method is applicable to various polyamide fibres and blended product thereof, and its form is fiber, yarn, fabric or nonwoven fabrics.
Beneficial effect
1. oxidation Acid system of the present invention is cleared up thoroughly, fully the polyamide fibre oxidation, has avoided the interference of organic compound to testing result, provides favourable basis to the detection of microscale harmful substance in the textile; Be applicable to the sample pre-treatments before objectionable impurities detects in the various polyamide fibre goods goods;
2. this oxidation Acid system can make polyamide fibre thoroughly clear up, and has efficient height, the simple, convenient characteristics cleared up.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Getting concentration is potassium bichromate solution 10ml, the distilled water 30ml of 0.7000mol/L, a small amount of zeolite and polyamide fibre sample 0.0150g, the capacity that joins successively is in the ground conical flask of 250ml, said vesse is placed cooling bath, get again pre-configured silver sulfate and sulfuric acid mixture liquid (Ag
2SO
4: H
2SO
4=1: 3V/V) 30ml, under the condition of low rate mixing, slowly join in the container, connect spherical condensation tube and connect flow condensation water, open thermal source, the digestion solution in the bottle is heated to boils, timing, digestion time is from the digestion solution boiling 2 hours.During clearing up, adjusting adds heat and keeps digestion solution to be slight boiling condition.Clear up end, digestion solution is poured onto in the clean glass beaker, with distilled water digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into.Glass beaker is placed in the cooling bath, slowly add potassium hydroxide 65g and make it to be neutralized to neutrality;
Embodiment 2
Getting concentration is potassium bichromate solution 15ml, the distilled water 30ml of 0.6500mol/L, a small amount of zeolite and polyamide fibre sample 0.0200g, the capacity that joins successively is in the ground conical flask of 250ml, said vesse is placed cooling bath, get again pre-configured silver sulfate and sulfuric acid mixture liquid (Ag
2SO
4: H
2SO
4=1: 3V/V) 30ml, under the condition of low rate mixing, slowly join in the container, connect spherical condensation tube and connect flow condensation water, open thermal source, the digestion solution in the bottle is heated to boils, timing, digestion time is from the digestion solution boiling 2 hours.During clearing up, adjusting adds heat and keeps digestion solution to be slight boiling condition.Clear up end, digestion solution is poured onto in the clean glass beaker, with distilled water digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into.Glass beaker is placed in the cooling bath, slowly add potassium hydroxide 50g g and make it to be neutralized to neutrality;
Embodiment 3
Getting concentration is potassium bichromate solution 10ml, the distilled water 30ml of 0.9000mol/L, a small amount of zeolite and polyamide fibre sample 0.0200g, join successively in the round-bottomed flask that capacity is 300ml, said vesse is placed cooling bath, get again pre-configured silver sulfate and sulfuric acid mixture liquid (Ag
2SO
4: H
2SO
4=1: 3V/V) 30ml, under the condition of low rate mixing, slowly join in the container, connect spherical condensation tube and connect flow condensation water, open thermal source, the digestion solution in the bottle is heated to boils, timing, digestion time is from the digestion solution boiling 2 hours.During clearing up, adjusting adds heat and keeps digestion solution to be slight boiling condition.Clear up end, digestion solution is poured onto in the clean glass beaker, with distilled water digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into.Glass beaker is placed in the cooling bath, slowly add potassium hydroxide 65g g and make it to be neutralized to neutrality;
Embodiment 4
Getting concentration is potassium bichromate solution 80ml, the distilled water 80ml of 1.5000mol/L, a small amount of zeolite and polyamide fibre sample 0.5000g, the capacity that joins successively is in the ground round-bottomed flask of 500ml, said vesse is placed cooling bath, get again pre-configured silver sulfate and sulfuric acid mixture liquid (Ag
2SO
4: H
2SO
4=1: 3V/V) 200ml, under the condition of low rate mixing, slowly join in the container, connect spherical condensation tube and connect flow condensation water, open thermal source, the digestion solution in the bottle is heated to boils, timing, digestion time is from the digestion solution boiling 2 hours.During clearing up, adjusting adds heat and keeps digestion solution to be slight boiling condition.Clear up end, digestion solution is poured onto in the clean glass beaker, with distilled water digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into.Glass beaker is placed in the cooling bath, slowly add potassium hydroxide 420g and make it to be neutralized to neutrality;
Claims (8)
1. the oxidizing digestion method of a polyamide fibre comprises:
Get the potassium bichromate solution that 5.0～100ml concentration is 0.5000～1.5000mol/L, 20～150ml water, zeolite and 0.0100～1.0000g polyamide fibre sample, join successively in the container, container is placed cooling bath, get silver sulfate and sulfuric acid mixture liquid, under low rate mixing, slowly join in the container, connect spherical condensation tube and connect flow condensation water, open thermal source, digestion solution in the bottle is heated to boils, adjusting adds heat and keeps digestion solution to be slight boiling condition 2-3 hour, clear up end, be poured onto in the clean glass beaker, with distilled water digestion container cleaned 3-5 time, collect cleaning fluid and incorporate digestion solution into, glass beaker is placed in the cooling bath, slowly add alkaline matter and make digestion solution be neutralized to neutrality;
Described thermal source is a kind of in natural gas, artificial water gas or the electrical heating, and heating-up temperature is 125～150 ℃.
2. the oxidizing digestion method of a kind of polyamide fibre according to claim 1 is characterized in that: the purity of above-mentioned used material is to be analyzed purely, and water is distilled water.
3. the oxidizing digestion method of a kind of polyamide fibre according to claim 1, it is characterized in that: the concentration of described potassium bichromate solution is 0.500～1.000mol/L.
4. the method cleared up of the oxidation of polyamide fibre according to claim 1, it is characterized in that: the mixing ratio of described silver sulfate and sulfuric acid mixture liquid is silver sulfate: sulfuric acid=1:3V/V.
5. the oxidizing digestion method of a kind of polyamide fibre according to claim 1 is characterized in that: described alkaline matter is solid-state or aqueous potassium hydroxide, NaOH in a kind of, its purity level is pure for analyzing.
6. the oxidizing digestion method of a kind of polyamide fibre according to claim 1 is characterized in that: digestion instrument is comprised of ground conical flask or round-bottomed flask, spherical reflux condensing tube, gas burning lamp or electric furnace, asbestos gauge, iron stand.
7. the oxidizing digestion method of a kind of polyamide fibre according to claim 1, it is characterized in that: clear up product and detect through elemental analyser, the detected level of carbon, nitrogen element can be lower than 0.05%.
8. described method is characterized in that according to claim 1～8, the method be applicable to polyamide fibre through purely spin, blending, the textile fabrics that interweaves and make, its form comprises fiber, yarn, fabric or nonwoven fabrics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910054388 CN101598722B (en) | 2009-07-03 | 2009-07-03 | Oxidizing digestion method for polyamide fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910054388 CN101598722B (en) | 2009-07-03 | 2009-07-03 | Oxidizing digestion method for polyamide fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101598722A CN101598722A (en) | 2009-12-09 |
| CN101598722B true CN101598722B (en) | 2013-01-02 |
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|---|---|---|---|
| CN 200910054388 Expired - Fee Related CN101598722B (en) | 2009-07-03 | 2009-07-03 | Oxidizing digestion method for polyamide fiber |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102187868B (en) * | 2010-03-03 | 2014-07-02 | 中农立华生物科技股份有限公司 | Flubendiamide and emamectin benzoate blended emulsion and preparation method thereof |
| CN102323137B (en) * | 2011-09-07 | 2013-01-23 | 中国农业科学院草原研究所 | Fiber digestion apparatus |
| CN104374868B (en) * | 2014-11-27 | 2016-04-06 | 中国石油天然气股份有限公司 | Method for detecting content of microsphere mobile gel in produced liquid and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2739612Y (en) * | 2004-10-10 | 2005-11-09 | 季克和 | High temperature dispelling instrument |
| CN101446558A (en) * | 2008-12-23 | 2009-06-03 | 天津创业环保集团股份有限公司 | Digestion solution for monitoring chemical oxygen demand in sewage |
-
2009
- 2009-07-03 CN CN 200910054388 patent/CN101598722B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2739612Y (en) * | 2004-10-10 | 2005-11-09 | 季克和 | High temperature dispelling instrument |
| CN101446558A (en) * | 2008-12-23 | 2009-06-03 | 天津创业环保集团股份有限公司 | Digestion solution for monitoring chemical oxygen demand in sewage |
Non-Patent Citations (1)
| Title |
|---|
| 李荣福等.《聚酰胺热氧化降解机理》.《高分子学报》.2000,(第2期),136-141. * |
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