JPH08178875A - Method for measuring concentration of rubber adhesion prevention agent - Google Patents

Abstract

PURPOSE: To measure the concentration quickly with high accuracy, prevent the overuse of a rubber adhesion prevention agent, reduce the cost and restrict pollution to the environment at a work place by quantitatively analyzing potassium ions in the liquid rubber adhesion prevention agent by an X-ray fluorescence analysis. CONSTITUTION: A liquid rubber adhesion prevention agent 2 is obtained by diluting a soap agent 5 including soft soap and metal soap with water. An X-ray fluorescence analyzer 13 has an X-ray projector for casting first-order X rays on a specimen on a sample 12, a spectroscope for analyzing spectra of second-order fluorescent X rays generated from the specimen, and a measuring device for measuring the intensity of fluorescent X rays of a wavelength corresponding to the potassium from the spectral analysis. A control means 9 is provided with an operating device which, when receiving the intensity of fluorescent X rays of the potassium measured (13), converts the intensity into the concentration of the rubber adhesion prevention agent 2. When the converted value is outside a proper concentration range of the rubber adhesion prevention agent 2, e.g. 0.5-5.0%, the control means 9 sends a signal to supply a suitable amount of the soap agent 5 and a diluent water 6 to a concentration-adjusting means 7.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention can measure the concentration of a liquid rubber anti-adhesive agent quickly and with high accuracy, and can reduce the cost in the rubber industry and prevent pollution of the work environment. Regarding measurement method.

[0002]

2. Description of the Related Art Generally, in the production of rubber products, in order to impart predetermined elastic properties to rubber, the rubber is plasticized by mastication prior to the molding and vulcanization process. A kneading operation is performed in which compounding agents such as a vulcanizing agent, a vulcanization accelerator, and a filler are uniformly kneaded. Also, for this kneading work,
Normally, a closed kneader such as a Banbury machine is used,
In this closed kneader, the kneading rubber is kneaded at a high temperature because the kneading is carried out at a high temperature in order to increase the mixing efficiency. Therefore, in order to prevent the kneaded rubber from adhering to each other due to the high temperature and the generation of scorch due to residual heat, the kneaded rubber is mixed with a liquid rubber anti-adhesive agent prior to the molding and vulcanization process. It is necessary to coat the rubber surface with a rubber anti-adhesion agent at the same time as cooling it.

On the other hand, a rubber anti-adhesive agent is generally a liquid obtained by diluting a soap agent containing water-soluble soft soap and water-insoluble metal soap with water, and the concentration of this soap agent is shown in FIG. 2 shows the correlation between the rubber anti-adhesive agent concentration and the anti-adhesion effect of rubber. As shown in the figure, although an increase in the concentration of the rubber anti-adhesive agent enhances the anti-adhesion effect of rubber, an excessive increase in the concentration, on the contrary, reduces the degree of increase in the anti-adhesion effect and causes an increase in cost. It causes harmful effects such as inducing dirt in the work environment,
Therefore, it is desirable to use the rubber anti-adhesive agent in a concentration range of 0.5 to 5%.

Conventionally, in order to control and control the rubber anti-adhesive agent within this concentration range, the liquid rubber anti-adhesive agent is sampled and the amount of the solid component obtained by drying the liquid anti-adhesive agent is measured to obtain the liquid rubber. The concentration of the anti-adhesive was calculated.

[0005]

However, in such a conventional measuring method, a large amount of time is required for heating and drying the sample, and the measuring efficiency is poor. Moreover, since the metal soap, which is the main part of the solid component, is non-water-soluble, the dispersion becomes non-uniform, such as suspension in a state in which the upper part of the liquid is thin and the lower part is thick, which impairs measurement accuracy and increases reliability. It was lacking.

In view of such a situation, the present inventor has further studied the relationship between the components of the rubber anti-adhesive agent and the anti-adhesion effect of rubber. As a result, 1) the component that affects the anti-adhesion effect is essentially soft soap, and 2) the rubber anti-adhesive agent by detecting the concentration of potassium ion in the soft soap dissolved in water. The inventors of the present invention have found that the concentration measurement can be performed accurately and quickly, and that 3) potassium ions in a liquid can be quantitatively analyzed by a fluorescent X-ray analysis method.

That is, the present invention is based on the quantitative analysis of potassium ion of a liquid rubber anti-adhesive agent by a fluorescent X-ray analysis method, and the concentration of the rubber anti-adhesive agent can be measured rapidly and with high accuracy, and an excessive rubber content can be obtained. The purpose of the present invention is to provide a method for measuring the concentration of a rubber anti-adhesive agent, which can prevent the use of the anti-adhesive agent, reduce costs, and prevent pollution of the work environment.

[0008]

The present invention provides a method for measuring the concentration of a liquid rubber anti-adhesive agent obtained by diluting a soap containing water-soluble soft soap and water-insoluble metal soap with water. ,
A method for measuring the concentration of a rubber anti-adhesive agent, which comprises quantitatively analyzing potassium ions of the liquid rubber anti-adhesive agent by a fluorescent X-ray analysis method.

In the quantitative analysis, a solution body from which water-insoluble metal ions are removed by pressure filtration of the liquid rubber anti-adhesive agent is taken out, and the solution body is adsorbed on a filter paper. It is preferable to carry out.

[0010]

Function: The index of the concentration of the liquid rubber anti-adhesive agent is replaced with potassium ion in the soft soap. As described above, the component that affects the rubber anti-adhesion effect is essentially soft soap, and therefore, by measuring the concentration of potassium ion in the liquid rubber anti-adhesive agent, the liquid rubber anti-adhesion agent can be measured. The concentration of the agent can be accurately controlled from the viewpoint of anti-adhesion effect.

Since the soft soap is water-soluble and the potassium ions are uniformly dispersed throughout the solution,
Even with a small amount and arbitrary sampling, it is possible to grasp the concentration of the rubber anti-adhesive agent in the entire solution, and the accuracy and reliability can be improved.

Further, since potassium ions are quantitatively analyzed by the fluorescent X-ray analysis method without requiring a step such as heating and drying, rapid and highly accurate measurement is possible.

The fluorescent X-ray analysis method uses the principle that when a sample is excited by irradiation with primary X-rays, the sample generates secondary fluorescent X-rays of a specific wavelength according to the elements in the sample. Therefore, more specifically, the generated fluorescent X-rays are spectrally analyzed by a spectrometer, and the intensity of the analysis spectrum of the wavelength of the fluorescent X-rays corresponding to a predetermined element, potassium in the present application, is measured to determine the intensity of potassium. Perform quantitative analysis. The intensity of the analysis spectrum is generally proportional to the amount of the predetermined element. For this purpose, the intensity of the primary X-rays irradiated to the predetermined element is constant, and the predetermined element is uniform on the sample surface. Must be attached to. However, since the water-insoluble metal soap is suspended in the liquid rubber anti-adhesive agent, the particles of the metal soap diffusely reflect the primary X-rays,
Irradiation intensity of a given element of primary X-rays is changed nonuniformly. Therefore, in the quantitative analysis, it is preferable to take out the solution body which is a sample from which the metal soap has been removed by pressurizing the liquid rubber anti-adhesive agent under pressure, and by adsorbing this solution body on the filter paper, It becomes possible to adhere potassium constantly to the surface of the filter paper. This allows more accurate concentration measurement.

[0014]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings, taking as an example the case of being applied to a concentration control device for a rubber anti-adhesive agent. FIG. 1 schematically shows a concentration control device 1 for a rubber deposition preventive agent. As shown in FIG. 1, the concentration control device 1 includes a cooling tank 3 in which a liquid rubber anti-adhesive agent 2 is stored, a concentration measuring unit 4 for measuring the concentration of the rubber anti-adhesive agent 2 in the cooling tank 3, and the cooling device. Tank 3
To the concentration adjusting means 7 for supplying the concentration adjusting soap 5 and the dilution water 6 and the measurement result by the concentration measuring means 4 to supply the appropriate amount of the soap 5 and the dilution water 6 from the concentration adjusting means 7. And a control means 9 for making it.

The liquid rubber anti-adhesive 2 is obtained by diluting a soap agent containing a soft soap and a metal soap with water. The soap agent includes, in addition to the soft soap and the metal soap, It contains auxiliary agents such as penetrants and surfactants. Also, soft soap is
The higher fatty acid potassium salt is water-soluble, and the metal soap is a metal salt of a higher fatty acid such as aluminum, manganese, or calcium other than the alkali salt, and is water-insoluble and dispersed in water. A suspension is formed.

The concentration measuring means 4 includes an introduction pipe 10 for collecting the liquid rubber anti-adhesion agent 2 for concentration measurement from the cooling tank 3 by a suction pump and the like, and a liquid rubber anti-adhesion product taken by the introduction pipe 10. Filter 11 for filtering agent 2 under pressure
A pressure filter 11 having A, and the filtration filter 11A
The sample 12 for concentration measurement is prepared by adsorbing the solution body 12A pressure-filtered by the method on the filter paper 12B. Further, the concentration measuring means 4 further includes the sample 12
An X-ray fluorescence analyzer 13 is provided for performing X-ray fluorescence analysis on the potassium adsorbed on.

The pressurizing machine 11 removes insoluble matter mainly composed of metal soap from the liquid rubber anti-adhesive agent 2 by pressurizing filtration, whereby the primary X-rays in the fluorescent X-ray analysis method are insoluble in water. It is possible to prevent irregular reflection on the particles having a certain property, and to ensure that the sample 12 is irradiated with the primary X-rays with a constant intensity. Therefore, the filtration filter 11A has, for example, 0.45 μm.
Those having a filtration capacity of about m can be preferably used.

Further, the filter paper 12B for preparing the sample 12 is a normal paper filter, for example, No. As the sample 12, one drop (about 1 cc) of the solution body 12A as a sample is adsorbed on the filter paper 12B to diffuse the solution body 12A into a circular shape having a diameter of about 3 cm. The maximum measurement range of the fluorescent X-ray analyzer 13 is generally about 5 cm in diameter, and therefore the total amount of potassium contained in one drop of the solution body is the measurement target, and high measurement accuracy is ensured.

The fluorescent X-ray analyzer 13 is an X-ray irradiator for irradiating the sample on the sample 12 with primary X-rays, and a spectrometer for spectrally analyzing secondary fluorescent X-rays generated from the sample. A turntable for measuring the intensity of fluorescent X-rays having a wavelength corresponding to potassium from spectrum analysis, and in this example, a plurality of, for example, 40 to 60 samples 12 are sequentially supplied to the irradiation position of the primary X-rays. Feeding stand 1
3A is attached.

The control means 9 includes the fluorescent X-ray analyzer 1
The fluorescent X-ray intensity of potassium measured by 3 is received, and an arithmetic unit for converting this fluorescent X-ray intensity of potassium into the concentration of the rubber anti-adhesive agent is provided. When it is out of the range, for example, 0.5 to 5.0%, a signal is sent to the concentration adjusting means 7 to supply appropriate amounts of the soap agent 5 and the diluting water 6.

The concentration adjusting means 7 comprises reservoirs 7A and 7B for storing the soap 5 and the diluting water 6, respectively, and the reservoirs 7A and 7B are supplied to the reservoirs 7A and 7B by a signal transmitted from the control means 9. A metering pump 15A having a solenoid valve for cutting and supplying appropriate amounts of the soap agent 5 and the dilution water 6 respectively.
5B is connected.

The concentration of the rubber anti-adhesive agent was changed by increasing the dilution water stepwise, and the change in the fluorescent X-ray intensity of potassium at that time measured with an X-ray fluorescence analyzer and the heating and drying were conducted. The relationship with the change in the weight of the measured solid component is shown in FIG. As shown in FIG. 2, the fluorescent X-ray intensity with potassium as an index is approximately directly proportional to the weight of the solid component, and thus it can be confirmed that the concentration of the rubber-proofing agent can be accurately measured by the fluorescent X-ray intensity of potassium.

FIG. 3 shows the relationship between the fluorescent X-ray intensity of potassium and the concentration of the rubber anti-adhesive agent, which the present inventor has learned. Based on the relationship shown in FIG. Conversion to the concentration of the anti-adhesive agent is performed.

[0024]

INDUSTRIAL APPLICABILITY As described above, the method for measuring the concentration of the rubber anti-adhesive agent of the present invention is such that the index of the concentration of the rubber anti-adhesive agent is replaced with potassium ion in the soft soap, and this potassium ion is analyzed by fluorescent X-ray analysis. Quantitative analysis by method. Therefore, the concentration can be measured quickly, reliably and highly accurately, and it is possible to prevent the excessive use of the rubber anti-adhesive agent, reduce the cost and suppress the pollution of the work environment.

[Brief description of drawings]

FIG. 1 is a schematic diagram showing an example of a concentration control device for a rubber deposition preventive agent for carrying out the present invention.

FIG. 2 is a diagram showing the relationship between the fluorescent X-ray intensity of potassium and the weight of solid components.

FIG. 3 is a diagram showing the relationship between the fluorescent X-ray intensity of potassium and the rubber anti-adhesive agent concentration.

FIG. 4 is a diagram showing the relationship between the rubber anti-adhesive agent concentration and the rubber anti-adhesion effect.

[Explanation of symbols]

 2 Rubber anti-adhesive 5 Soap 6 Water 11A Filtration filter 12 Sample 12A Solution body 12B Filter paper

Claims (2)

[Claims] 1. A method for measuring the concentration of a liquid rubber anti-adhesion agent obtained by diluting a soap agent containing water-soluble soft soap and non-water-soluble metal soap with water, wherein the liquid rubber anti-adhesion agent is used. A method for measuring the concentration of a rubber anti-adhesive agent, which is characterized by quantitatively analyzing the potassium ion of 1. by a fluorescent X-ray analysis method. 2. In the quantitative analysis, a solution body from which a water-insoluble metal soap is removed by pressure filtration of the liquid rubber anti-adhesive agent is taken out, and a sample obtained by adsorbing the solution body on a filter paper is taken out. The method for measuring the concentration of a rubber anti-adhesive agent according to claim 1, wherein the method is used.