Method for determining content of saturates, wax and oil in rubber and rubber auxiliaries

A technology of rubber additives and determination methods, applied in the field of testing and analysis, can solve the problems of small amount of wax added, brittleness, mutual interference in analysis, etc., and achieve the effects of fast column passing speed, high accuracy and simple operation.

Active Publication Date: 2017-12-29
SINO LEGEND CHINA CHEM +1
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Problems solved by technology

[0006] In the analysis of components of rubber products and testing of raw materials, the analysis and quantification of oil and wax have always been a concern in the industry. However, since wax and oil are usually mixed in rubber and rubber additives, the composition of oil is relatively complicated. , and the amount of wax added is small, and they have similar molecular structures, which interfere with each other during analysis, and cannot be accurately quantified
[0007] Although the petrochemical industry has issued a variety of methods for separating saturated components, aromatic components, colloids, asphaltenes and waxes in petroleum products (such as asphalt, petroleum, oilfield sludge, etc.) by using alumina chromatography columns, but due to the The adsorption / desorption selectivity of the column for each component is weak, the amount of packing required to meet the separation capacity is large, and the column length is long, usually a glass tube of 40-70 cm; and the washing of the components needs to be completed under heating conditions. For deseparation, heating in a water bath at around 50°C is generally adopted, and the design of the chromatographic column is complicated, usually in the form of a sleeve, which is inconvenient to operate and fragile
Moreover, the amount of sample loaded by this method is relatively large (about 10g sample amount), which is not suitable for the separation and quantification of oil and wax in rubber products.
Because the total amount of oil and wax in rubber products is less than 10%, if you want to ensure the loading of 10g on the chromatography column, you need to process about 100g of rubber products, which is not possible for rubber products with a weight of only a few grams
[0008] In addition, the separation of wax in the petrochemical industry requires multiple steps such as dewaxing solvent, freeze crystallization, and vacuum drying. However, the trace amount of wax in rubber products cannot be obtained by freeze crystallization at all. Even if it crystallizes out, the amount obtained is far less than the loss. Therefore, the crystal weighing method is not suitable for the analysis and quantification of trace waxes in rubber products.

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  • Method for determining content of saturates, wax and oil in rubber and rubber auxiliaries
  • Method for determining content of saturates, wax and oil in rubber and rubber auxiliaries
  • Method for determining content of saturates, wax and oil in rubber and rubber auxiliaries

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Experimental program
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Embodiment 1

[0064] Embodiment 1: the determination of wax and oil in known sample

[0065] 1.1 Preparation of known samples

[0066] Mix raw materials T110, 4020, RD, SP1068, OK1987, and P50 according to the following proportions, then heat and stir for 60 minutes to fully mix the raw materials and obtain samples with known wax and oil contents. The information of each raw material is shown in Table 1-1.

[0067] Table 1-1 Raw material information and ratio in known samples

[0068]

[0069] 1.2 Determination of saturated content in samples

[0070] 1.2.1 Column packing: Take a chromatographic column with an inner diameter of 1.0 cm and a height of 20 cm, weigh 2.0 g of silica gel (200-300 mesh) and put it in the chromatographic column; continue to weigh 1.5 g of clay adsorbent and put it in the chromatographic column On the upper layer of the column, a piece of glass wool is placed on top of the clay adsorbent. When filling, a rubber ball can be used to tap the outer wall of the col...

Embodiment 2

[0114] Embodiment 2: Change the column packing parameters and solvent B in the saturated content determination step, the sample loading and other test methods and steps remain unchanged, and continue the test, as follows:

[0115] 2.1 Determination of saturated content in samples

[0116] 2.1.1 Column packing: Take a chromatographic column with an inner diameter of 2.0cm and a height of 30cm, weigh 2.5g of silica gel (60-100 mesh) and put it in the chromatographic column; continue to weigh 2.0g of clay adsorbent and put it in the chromatographic column On the upper layer of the column, a piece of glass wool is placed on top of the clay adsorbent. When filling, a rubber ball can be used to gently tap the outer wall of the column to ensure that the adsorbent in the column has a similar density (the silica gel has been heated at 190°C for 4 hours to activate before loading the column).

[0117] 2.1.2 Weigh about 100mg of the sample into a 10ml volumetric flask, add 1ml of petrole...

Embodiment 3

[0129] Embodiment 3: the mensuration of saturated content in table tennis sponge film

[0130] 3.1 Sample extraction

[0131] 3.1.1 Crush the sponge film into a size of 1mm with a freeze grinder 3 For the left and right rubber powder particles, accurately weigh about 2g of rubber powder, wrap it with weighed filter paper, place it on a Soxhlet extraction device, and extract it with acetone for 8 hours.

[0132] 3.1.2 Remove the extracted sample from the Soxhlet extraction device, place the filter paper bag in an oven at 70°C for about 12 hours, and weigh the filter paper bag every 10 minutes. When the difference between the two weighings is 0.5 When it is within mg, it is considered that the solvent is completely removed, and the result of the second weighing is recorded.

[0133] 3.1.3 Transfer all the liquid in the extraction bottle to a pear-shaped bottle, wash the extraction bottle with clean acetone three times, transfer the solution into the pear-shaped bottle, and pla...

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Abstract

The invention provides a method for determining content of saturates, wax and oil in rubber and rubber auxiliaries. The method comprises the steps as follows: a solution containing rubber or rubber auxiliary samples or a solution containing rubber or rubber auxiliary sample extracts is added to a chromatographic column, the solution sequentially passes through a clay adsorbent layer and a silica gel layer in the chromatographic column, the solution passing through the chromatographic column is collected, saturates are obtained after a solvent in the collected solution is removed, an internal standard substance is added to the obtained saturates, the mass percentage of each alkene is calculated through gas chromatography test, the wax content is calculated, the difference between the wax content and the saturate content is the content of oil in the sample, the extracts are obtained after removal of the solvent from extract solution obtained through extraction of rubber and rubber auxiliary samples. The saturates in rubber products and rubber auxiliaries can be separated and quantified under the condition of normal temperature and extremely small loading quantity with the method.

Description

technical field [0001] The invention relates to a method for measuring saturated content, wax and oil content in rubber and rubber additives, and belongs to the technical field of testing and analysis. Background technique [0002] Oil and wax are very important raw materials in the rubber industry. They are all petroleum products. The main component of wax is C 20 The combination of the above normal alkanes and isoparaffins; the oil is divided into aliphatic hydrocarbon oil, naphthenic oil and aromatic hydrocarbon oil, and the proportions of chain hydrocarbons, naphthenic hydrocarbons and aromatic hydrocarbons in different types of oil are different. [0003] The hardness of the rubber itself is high, and the hardness of the rubber will be higher after adding fillers and rubber additives during the production process. Filling a certain amount of oil in the rubber can make it soft and have good elasticity. Synthetic rubber, especially Yes, styrene-butadiene rubber is usuall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 高剑琴房彩琴赵丽丽刘慧娜张成董栋
Owner SINO LEGEND CHINA CHEM
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