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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- insoluble sulfur
- differential thermal
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- ageing
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Abstract
The present invention relates to intermediate product testing technology which is used for testing whether the ageing is complete in the process of preparing insoluble sulfur or not, particularly to an ageing process testing method in the process of preparing insoluble sulfur by differential thermal analysis technology. A differential thermal analysis method is used, air is used as a testing atmosphere, and the testing temperature is from 20 to 200 DEG C. By testing a differential thermal analysis curve of an ageing sample, the present invention is used for testing whether the ageing sample has an obvious exothermic peak within the temperature of 30 to 160 DEG C or not so as to judge whether the ageing is complete or not. The present invention has good practicability, and can rapidly and accurately determine the ageing degree. In the process of preparing insoluble sulfur, the present invention uses differential thermal technology, the differential thermal peak change of the ageing product is utilized, the ageing progress is monitored in real time, and the purpose of controlling product quality is achieved.
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)
1. aging progress detection method in the insoluble sulfur preparation process, it is characterized in that: utilize differential thermal analysis, with the air is to detect atmosphere, detected temperatures is 20 ℃～200 ℃, by measuring the aged samples differential thermal analysis curve, observe it in 60 ℃～90 ℃, have or not and tangible exothermic peak occurs, judge aging whether complete.
2. whether according to aging progress detection method in the described insoluble sulfur preparation process of claim 1, it is characterized in that: described detected temperatures is 60 ℃～90 ℃, observes it have or not in 60 ℃～90 ℃ and tangible exothermic peak occurs, judge aging complete.
3. according to aging progress detection method in claim 1 or the 2 described insoluble sulfur preparation process, it is characterized in that: the specimen in the described testing process begins to heat up from being lower than detected temperatures, and programming rate is 1 ℃/minute～10 ℃/minute.
4. according to aging progress detection method in the described insoluble sulfur preparation process of claim 3, it is characterized in that: described programming rate is 4 ℃/minute～6 ℃/minute.
5. according to aging progress detection method in claim 1 or the 2 described insoluble sulfur preparation process, it is characterized in that: the specimen in the described testing process is to gather and sampling after ground and mixed is even from the different parts uniform stationing of aging equipment.
6. according to aging progress detection method in the described insoluble sulfur preparation process of claim 1, it is characterized in that: the instrument that utilizes differential thermal analysis to use is differential thermal analyzer.
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1553173A CN1553173A (en) | 2004-12-08 |
| CN1252465C true CN1252465C (en) | 2006-04-19 |
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| Application Number | Title | Priority Date | Filing Date |
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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
- 2003-06-04 CN CN 03133588 patent/CN1252465C/en not_active Expired - Fee Related
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