CN1252465C - Ageing progress testing method in insoluble sulfur preparing process - Google Patents
Ageing progress testing method in insoluble sulfur preparing process Download PDFInfo
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- CN1252465C CN1252465C CN 03133588 CN03133588A CN1252465C CN 1252465 C CN1252465 C CN 1252465C CN 03133588 CN03133588 CN 03133588 CN 03133588 A CN03133588 A CN 03133588A CN 1252465 C CN1252465 C CN 1252465C
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- Prior art keywords
- aging
- insoluble sulfur
- differential thermal
- thermal analysis
- detection
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Links
- 230000032683 aging Effects 0.000 title claims abstract description 42
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 32
- 239000011593 sulfur Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000012360 testing method Methods 0.000 title claims description 6
- 238000004455 differential thermal analysis Methods 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 18
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000013067 intermediate product Substances 0.000 abstract description 5
- 238000007689 inspection Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000005864 Sulphur Substances 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000002902 bimodal effect Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000007500 overflow downdraw method Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012430 stability testing Methods 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- -1 tire Polymers 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
本发明涉及检测不溶性硫磺制备过程中老化是否完全的中间产品检验技术，具体地说是一种利用差热分析技术不溶性硫磺制备过程中老化进度检测方法，利用差热分析方法，以空气为检测气氛，检测温度为20℃～200℃，通过测定老化样品差热分析曲线，观测其在30℃～160℃内有无出现明显的放热峰，判断老化是否完全。其实用性好，能快速、准确确定老化程度；在制备不溶性硫磺过程中，本发明使用差热技术，利用老化产品差热峰型变化，适时监空老化进度，达到控制产品质量的目的。The invention relates to an intermediate product inspection technology for detecting whether the aging is complete in the preparation process of insoluble sulfur, specifically a method for detecting the aging progress in the preparation process of insoluble sulfur using differential thermal analysis technology, using differential thermal analysis method, and using air as the detection atmosphere , the detection temperature is 20°C-200°C, by measuring the differential thermal analysis curve of the aging sample, observe whether there is an obvious exothermic peak within 30°C-160°C, and judge whether the aging is complete. It has good practicability and can quickly and accurately determine the degree of aging; in the process of preparing insoluble sulfur, the present invention uses differential heat technology to utilize the change of differential heat peak shape of aged products to monitor the aging progress in time to achieve the purpose of controlling product quality.
Description
Technical field
The present invention relates to detect aging whether completely intermediate product inspection technology in the insoluble sulfur preparation process, specifically a kind of progress detection method that wears out in the differential thermal analysis (DTA) technology insoluble sulfur preparation process of utilizing.
Background technology
Insoluble sulfur is the high molecular polymer of sulphur, gains the name because of it is insoluble to carbon disulphide, and insoluble sulfur is mainly used in rubbers such as tire, rubber overshoes, sebific duct, adhesive tape.
Be that method that raw material is produced insoluble sulfur has two kinds of fusion method and gasifications with sulphur.Insoluble sulfur preparation generally comprises that polymerization and aging, pulverizing and extraction, auxiliary agent are handled and technological process such as oil-filled; Wherein aging is the important intermediate link that whole insoluble sulfur is produced; In the insoluble sulfur production run, resulting viscoelasticity intermediate product behind the quenching, after aging thermal treatment, product becomes hard and crisp from form, and the polymerised sulphur molecule stereo structure changes on the microcosmic; Have only through suitable burin-in process, the insoluble sulfur final products just can have thermal stability preferably; Burin-in process is incomplete, and then the thermally-stabilised rate of final products is low, and burin-in process is excessive, and product yield is reduced.
Now, in the relevant document of insoluble sulfur preparation both at home and abroad, production, all find no the report that closes detection method in the burin-in process.
Summary of the invention
The object of the present invention is to provide aging progress detection method in a kind of insoluble sulfur preparation process of fast, accurately determining degree of aging.
For achieving the above object, the technical solution used in the present invention is:
Whether utilizing differential thermal analysis, is to detect atmosphere with the air, and detected temperatures is 20 ℃～200 ℃, by measuring the aged samples differential thermal analysis curve, observes it have or not in 30 ℃～160 ℃ and tangible exothermic peak occurs, judge aging complete; In 30 ℃～160 ℃ analystal sections, compare with aging sample differential thermal curve completely, a tangible exothermic peak is arranged on the unaged differential thermal curve of sample completely.
Be fast detecting, the detected temperatures scope can be contracted between 60 ℃～90 ℃; Observe it in 60 ℃～90 ℃, have or not and tangible exothermic peak (requiring its instrument detecting precision height this moment) occurs, judge aging whether complete; Unaged sample characteristic completely peak appears between 60 ℃-90 ℃, and it is an exothermic peak, and peak shape is unimodal or bimodal.
Specimen in the described testing process begins to heat up from being lower than detected temperatures, and programming rate is 1 ℃/minute～10 ℃/minute, but in order to improve accuracy of detection and to accelerate detection speed, the differential thermal analyzer programming rate preferably is controlled to be 4 ℃/minute～6 ℃/minute;
Representative for guaranteeing test sample, test sample should be gathered and sampling after ground and mixed is even at the different parts uniform stationing of aging equipment; Sampling quantity is decided according to the aging equipment production scale, generally can be optional between 5 grams～100 grams, and the specimen weighing amount is generally between 10 milligrams～50 milligrams; The instrument that the present invention uses is mainly differential thermal analyzer;
Concrete detection method is: at first get a certain amount of aging insoluble sulfur sample and be put in the differential thermal analyzer sample cell, connecting air begins by certain speed intensification heating, follow the tracks of and detect the thermal analysis curue spectrum, see whether it tangible exothermic peak occurs in 30 ℃～160 ℃ scopes, as do not have the exothermic peak appearance, prove that then sample is fully aging.
The present invention promptly can be used for vapor phase method and also can be used for fusion method and prepare in the Manufacture of insoluble sulphur process; Above-mentioned agingly be meant that the elastic sulfur behind the quenching is heat treatment process at a certain temperature in the process of producing insoluble sulfur, after this thermal treatment, product form becomes the fragility body by viscoelastic body; The purpose of carrying out burin-in process in the insoluble sulfur production run mainly is in order to improve the thermal stability of final products.
The present invention has following advantage:
1. practicality is good.Adopting the present invention to control production can make the insoluble sulfur product of being produced have higher thermally-stabilised rate.In preparation insoluble sulfur process, an aging step is to the final mass-heat-resistant stability of insoluble sulfur product, and product yield plays an important role; Aging not exclusively then product poor heat stability; Overaging can reduce product yield again; The present invention uses the differential thermal technology, utilizes ageing prod differential thermal peak type to change, and supervises empty aging progress in good time, reaches the purpose of control product quality.
2. fast, accurately determine degree of aging.The present invention can obtain the qualitative conclusion of insoluble sulfur aging of product degree in a few minutes to tens minutes time.
Description of drawings
Fig. 1 is the differential thermal analysis curve of aging complete sample;
Fig. 2 is the differential thermal analysis curve of unaged complete sample.
Embodiment:
Embodiment 1
100 kilograms of treatment capacities/batch box burin-in process device in, a batch sample under certain temperature aging 3 hours; At 5 different parts of this batch sample respectively take a sample respectively 5 grams, altogether sample thief 25 grams; After mixing, therefrom take by weighing 25 milligrams of samples and put into the differential thermal analyzer sample cell, with the air is to detect atmosphere, from 50 ℃, programming rate with 5 ℃ of per minutes is warming up to 160 ℃, detects the differential thermal analysis (DTA) collection of illustrative plates simultaneously, only detects a strong endothermic peak and an exothermic peak in the differential thermal collection of illustrative plates of this sample, wherein the exothermic peak peak value is about 115 ℃, and the endothermic peak peak value is about between 125 ℃; No exothermic peak occurs between 60 ℃～90 ℃, illustrates that this batch aged samples is fully aging.
With the aging intermediate product of this batch, through further handling, the insoluble sulfur product that finally makes carries out heat stability testing through at 110 ℃ under 15 minutes conditions, and thermally-stabilised rate is 85.6%.The analysis collection of illustrative plates of this batch aged samples is seen differential thermal analysis (DTA) Fig. 1.
Embodiment 2
With embodiment 1 the same manner aging 1 hour sample of another batch in the ager is carried out differential thermal analysis (DTA); Found that that a tangible heat release is arranged in its differential thermal collection of illustrative plates is bimodal between 60 ℃～90 ℃, illustrate that this batch product is unaged fully, the insoluble sulfur product that makes after method is similarly to Example 1 further handled with these intermediate product is through between 110 ℃, carry out heat stability testing under 15 minutes conditions, its thermally-stabilised rate is 71.3%.The analysis collection of illustrative plates of this batch aged samples is seen differential thermal analysis (DTA) Fig. 2.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133588 CN1252465C (en) | 2003-06-04 | 2003-06-04 | Ageing progress testing method in insoluble sulfur preparing process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133588 CN1252465C (en) | 2003-06-04 | 2003-06-04 | Ageing progress testing method in insoluble sulfur preparing process |
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| Publication Number | Publication Date |
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| CN1553173A CN1553173A (en) | 2004-12-08 |
| CN1252465C true CN1252465C (en) | 2006-04-19 |
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| CN 03133588 Expired - Fee Related CN1252465C (en) | 2003-06-04 | 2003-06-04 | Ageing progress testing method in insoluble sulfur preparing process |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102087233B (en) * | 2009-12-04 | 2013-08-21 | 复旦大学 | Method for characterizing progress and conversion rate of chemical reaction |
| CN104089848A (en) * | 2014-07-30 | 2014-10-08 | 合肥工业大学 | Method for detecting self safety of polyurethane grouting reinforcement material for underground coal mine in use process |
| CN105044150B (en) * | 2015-08-11 | 2017-11-03 | 山东金科力电源科技有限公司 | The method for detecting additive mixture homogeneity in polar plate of lead acid storage battery |
| KR102129582B1 (en) * | 2018-11-13 | 2020-07-02 | 넥센타이어 주식회사 | Analysis method for insoluble sulphur based material and method for manufacturing tire |
| KR102284797B1 (en) * | 2019-12-31 | 2021-08-03 | 넥센타이어 주식회사 | Analysis method for sulphur based tire material and method for manufacturing tire |
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- 2003-06-04 CN CN 03133588 patent/CN1252465C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1553173A (en) | 2004-12-08 |
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Granted publication date: 20060419 Termination date: 20100604 |