CN101598722A - A kind of oxidizing digestion method of polyamide fibre - Google Patents

A kind of oxidizing digestion method of polyamide fibre Download PDF

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Publication number
CN101598722A
CN101598722A CNA2009100543882A CN200910054388A CN101598722A CN 101598722 A CN101598722 A CN 101598722A CN A2009100543882 A CNA2009100543882 A CN A2009100543882A CN 200910054388 A CN200910054388 A CN 200910054388A CN 101598722 A CN101598722 A CN 101598722A
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polyamide fibre
digestion
solution
oxidizing
water
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CN101598722B (en
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王建庆
雷宁
李戎
林丹丽
黄劲旭
王改侠
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Donghua University
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Donghua University
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Abstract

The present invention relates to a kind of oxidizing digestion method of polyamide fibre, comprise: get potassium bichromate solution, water, zeolite and polyamide fibre sample, place cooling bath, get silver sulfate and sulfuric acid mixture liquid, under stirring at a slow speed, slowly join in the container, connect spherical condensation tube and connect flow condensation water, digestion solution in the bottle is heated to boils, clear up end, be poured onto in the clean glass beaker, clean, 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.The present invention clears up the polyamide fibre exhaustive oxidation to be simple compounds, to clear up product and detect through elemental analyser that the detected level of carbon, nitrogen element is lower than 0.05%, is applicable to the processing of clearing up of sample before micro substance detects in the textile.

Description

A kind of oxidizing digestion method of polyamide fibre
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 the laws and regulations and the associated documents of ecological textile aspects such as OEKOTEX STANDARD 100, REACH rules; the Chinese government has also issued corresponding regulations and standard; yet China reaches in the world and still be at present blank relatively 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 be sought different extractants, and testing result is subjected to the influence 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, influences 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, clear up system by custom-designed oxidation, make polyamide fibre under certain condition exhaustive oxidation clear up and be simple compounds, avoided the interference of organic compound, provide favourable basis the detection of micro-objectionable impurities in the textile to testing result.This method is applicable to that objectionable impurities detects preceding sample pre-treatments in various polyamide fibres and the blended product thereof.
The invention provides a kind of oxidizing digestion method of polyamide fibre, comprise the steps:
Clear up system by the chemical oxidation that potassium dichromate, sulfate, sulfuric acid and the water of silver are formed, 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 of forming by ground conical flask or round-bottomed flask, spherical reflux condensing tube, combustion gas lamp or electric furnace, asbestos gauge, iron stand; Connect the cold water that flows in the shape reflux condensing tube of receiving on ground conical flask or the round-bottomed flask bottleneck, condenser pipe;
Digestion solution is formed:
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 pre-configured silver sulfate and sulfuric acid mixture liquid (Ag again 2SO 4: H 2SO 4=1: 3V/V) 15~150ml, slowly joining in the container under the stirring condition at a slow speed, 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 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.
This method is applicable to various polyamide fibres and blended product thereof, and its form is fiber, yarn, fabric or nonwoven fabrics.
Beneficial effect
1. system is cleared up in oxidation of the present invention, and the polyamide fibre oxidation is cleared up thoroughly, fully, has avoided the interference of organic compound to testing result, provides favourable basis to the detection of micro-objectionable impurities in the textile; Be applicable to the sample pre-treatments before objectionable impurities detects in the various polyamide fibre goods goods;
2. this oxidation is cleared up system polyamide fibre is thoroughly cleared 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 to the present invention is described 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 institute restricted portion 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 of joining is in the ground conical flask of 250ml successively, said vesse is placed cooling bath, get pre-configured silver sulfate and sulfuric acid mixture liquid (Ag again 2SO 4: H 2SO 4=1: 3V/V) 30ml, slowly joining in the container under the stirring condition at a slow speed, 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 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, digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into distilled water.Glass beaker is placed in the cooling bath, slowly add potassium hydroxide 65g and make it to be neutralized to middle part;
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 of joining is in the ground conical flask of 250ml successively, said vesse is placed cooling bath, get pre-configured silver sulfate and sulfuric acid mixture liquid (Ag again 2SO 4: H 2SO 4=1: 3V/V) 30ml, slowly joining in the container under the stirring condition at a slow speed, 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 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, digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into distilled water.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, the capacity of joining is in the round-bottomed flask of 300ml successively, said vesse is placed cooling bath, get pre-configured silver sulfate and sulfuric acid mixture liquid (Ag again 2SO 4: H 2SO 4=1: 3V/V) 30ml, slowly joining in the container under the stirring condition at a slow speed, 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 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, digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into distilled water.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 of joining is in the ground round-bottomed flask of 500ml successively, said vesse is placed cooling bath, get pre-configured silver sulfate and sulfuric acid mixture liquid (Ag again 2SO 4: H 2SO 4=1: 3V/V) 200ml, slowly joining in the container under the stirring condition at a slow speed, 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 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, digestion container is cleaned three times, collect cleaning fluid and incorporate digestion solution into distilled water.Glass beaker is placed in the cooling bath, slowly add potassium hydroxide 420g and make it to be neutralized to neutrality.

Claims (9)

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 in the container successively, container is placed cooling bath, get silver sulfate and sulfuric acid mixture liquid, under stirring at a slow speed, 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, digestion container cleaned 3-5 time, collect cleaning fluid and incorporate digestion solution into distilled water, glass beaker is placed in the cooling bath, slowly add alkaline matter and make digestion solution be neutralized to neutrality.
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.
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 a 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 thermal source is a kind of in natural gas, artificial water gas or the electrical heating, and heating-up temperature is 125~150 ℃.
6. 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.
7. the oxidizing digestion method of a kind of polyamide fibre according to claim 1 is characterized in that: digestion instrument is made up of ground conical flask or round-bottomed flask, spherical reflux condensing tube, combustion gas lamp or electric furnace, asbestos gauge, iron stand.
8. 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%.
9. according to the described method of claim 1~8, it is characterized in that, this 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.
CN 200910054388 2009-07-03 2009-07-03 Oxidizing digestion method for polyamide fiber Expired - Fee Related CN101598722B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102187868A (en) * 2010-03-03 2011-09-21 中农立华生物科技股份有限公司 Flubendiamide and emamectin benzoate blended emulsion and preparation method thereof
CN102323137A (en) * 2011-09-07 2012-01-18 中国农业科学院草原研究所 Fiber digestion apparatus
CN104374868A (en) * 2014-11-27 2015-02-25 中国石油天然气股份有限公司 Detection method of movable microsphere gel content in produced fluid and application thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2739612Y (en) * 2004-10-10 2005-11-09 季克和 High temperature dispelling instrument
CN101446558B (en) * 2008-12-23 2010-11-03 天津创业环保集团股份有限公司 Digestion solution for monitoring chemical oxygen demand in sewage

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102187868A (en) * 2010-03-03 2011-09-21 中农立华生物科技股份有限公司 Flubendiamide and emamectin benzoate blended emulsion and preparation method thereof
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
CN102323137A (en) * 2011-09-07 2012-01-18 中国农业科学院草原研究所 Fiber digestion apparatus
CN104374868A (en) * 2014-11-27 2015-02-25 中国石油天然气股份有限公司 Detection method of movable microsphere gel content in produced fluid and application thereof
CN104374868B (en) * 2014-11-27 2016-04-06 中国石油天然气股份有限公司 A kind of Produced Liquid microballoon shake gels detection method of content and application thereof

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