Control method and control of oil and petrochemical products through chemical processing and methods of operational use of sensors based on quartz crystal microbalance

 

(57) Abstract:

The invention relates to performance management and monitoring of dosage, and in particular to methods and control of oil and petrochemical products through chemical processing, as well as to methods for operational use of sensors based on quartz crystal microbalance. According to the invention are used resonators with varying shear thickness, which simultaneously measure the deposition of mass and properties of the fluid, which can be used to control the processing of petroleum, petrochemical, systems and water purification systems. Special chemical products as additives can be accurately and instantly added to control the conditions defined by the cavities with the oscillations of the shear thickness. Resonators with varying shear thickness are piezoelectric crystals used in conjunction with the generation scheme that can determine the mass, as well as the viscosity and/or density of the fluid in contact with the piezoelectric surface. 5 C. and 16 h.p. f-crystals.

Adding chemical compounds for special purposes in a variety of manufacturing Sov. Adding in such processes of chemical compounds intended for processing, may contribute, among others, the slow process of deterioration of the oil, corrosion and pricing. These chemical compounds special purpose add-in processes with concentrations varying from a few parts per million to several percent. The dosage of the compounds is often determined by the regulatory process variations over time, which correspond to the addition of special chemical compounds. In the optimal case, the experts would like to correlate dose with changes in fluids process. However, the means for determining the dosage often requires a long time as an important process parameters will be many times to change, and will change significantly only for a very long time. For some processes, an appropriate definition of the correct dosage of special chemical compounds can take several months. Once installed, these dosages be a static value. This dosage does not increase or decrease when the quality deterioration, corrosion or speed Preobrazhensky special products or product of inferior quality, insufficiently processed chemical products for special purposes.

Examples of methods used to control the addition of special chemical compounds that include the use of analysis of a test sample, offline (out of process) testing of residual product, testing of residual polymer, an operational check of the pH level, the monitoring device for conductivity, etc., However these ways and many others, which are used for performance management and monitoring of dosage, are usually slow and not showing real-time changes in the process. Testing of residual products, for example, usually involves removing a sample of fluid from the process and the analysis of this sample separately from the process. Similarly, in the case of operational measures, such as sensors for pH and conductivity meters, limit of detection and discrepancies in many ways is too high to obtain accurate data to control the addition of special chemical products. That is, the sensitivity of operational tools is often not high enough to enable the operator to adjust the dosage of SP the different chemicals in industrial processes highly sensitive method, performed in situ, which provides feedback in real time about the status of the fluid in the process.

It is known the use of a microbalance using quartz crystals to measure the extent of fouling, scaling or loss of mass that occurs in carbon and water systems. These devices operate on the principle of excitation of the quartz crystal in contact with a fluid medium (liquid or vapour) to the resonance frequency, and then measuring the shift in resonant frequency due to the loss or accumulation of mass from the surface of the crystal. While the measurement of the mass of sediment solids, crystalline scale or deteriorating the quality of the products are successful, the applicant has discovered that conventional devices microbalance the quartz crystals are unreliable indicator of many phenomena that take place in aqueous and nonaqueous systems. Firstly, the normal quartz microbalance accurately measure the mass of amorphous deposition, for example, from biogarantie, or amorphous deposits of hydrocarbons on the surface of the processing and so on, Relying on traditional quartz microbalance for these types of measurements, you can get inaccurate which has been created to correct conditions which measure (control).

Examples of typical use microbalance the quartz crystal to measure the formation of crystalline scale in aqueous systems described in pending application for U.S. patent No. 08/421206 from 13.04.1995, the disclosure of which is included in this description by reference. While the device and methods described in the application 421206 work correctly and provide excellent control only in the case when the system is formed only of the crystal scale, found that this device does not work on systems which may be formed of amorphous scum or a combination of amorphous and crystalline scale. Further, devices of this type, which is described in the application 421206, cannot be applied to perception taking place in a fluid environment changes, such as increasing or decreasing the viscosity, increase or decrease the density, the presence of immiscible fluid, or the growth of amorphous sediment build-up inside the container containing the fluid.

Accordingly, the present invention relates to a method for measuring properties of substances and process threads, and more specifically to the measurement of viscosity and density of substances, and more specifically to tab of the present invention uses the device of the resonator oscillations of the shear thickness to determine the accumulation of mass, viscosity and/or density carbon solutions, vapors and mixtures, and determining the accumulation of mass, viscosity and/or density of the aqueous fluid. Using this method, you can get a quick accurate measurements instantly, and over time, which can be used to control the addition of chemicals to process and process variables in the system. Using the device of the resonator oscillations of the shear thickness, can be significantly improved handling of crude petroleum and chemical products through correct and timely uploads preventing the degradation of substances by layering emulsion as in the processing of wastewater and demulsification of crude oil, as well as at separation of emulsions formed during the processing of crude oil (e.g. desalination, demulsification, and some emulsions formed during the processing of hydrocarbons, for example, in the columns of cooling the ethylene furnaces) by the proper addition of dispersants or other additives, hydrocarbons and by adding a biocide treated regulating chemicals or stabilizers. Similarly, the device of the reason is Denia biological, inorganic or organic residue, or the device can be used for measuring the rate of corrosion occurring or in water or in a hydrocarbon system. The additional use of the device of the resonator oscillations of the shear thickness are disclosed below.

Prior art

The microbalance the quartz crystal, sometimes also referred to as piezoelectric sensors, is proposed for measuring the mass of the substance deposited from the fluid, viscosity of the flowing fluid, determine the rate of deposition of thin films, monitoring, etc., Partly successfully used quartz microbalance, measuring only shifts the resonance frequency, often give erroneous readings when used in industry under certain conditions. For example, quartz microbalance, which were excellent when measuring sticky solid scale, which in real terms is deposited on the crystal and DAMPS vibration of the crystal, often do not give the correct results in the deposition of amorphous or soft fouling (biological growth, amorphous inorganic crystals I. p.) on the same crystal. That's why these devices rely that is ontrol for the addition of chemical products, intended for processing, such as biocides and antiparasitary.

Resonators with varying shear thickness, useful in practice of the present invention, specialists known. Especially useful resonator oscillation shear thickness is disclosed in U.S. patent No. 5201215 issued Granstaff (Granstaff) and others, the disclosure of which is included in this description by reference. This device is able to determine the product of the density-viscosity of a given fluid. It should be noted that the quartz part of the resonator oscillations of the shear thickness is essentially identical to the known quartz crystal microbalance. There is a way in which process the signal, which gives the uniqueness of the use of resonators Granstaff to fluctuations in shear thickness, and which allows these resonators to fluctuations in shear thickness to do what ordinary quartz microbalance cannot do. Useful in this invention honours resonators with varying shear thickness from the quartz microbalance, which cannot be used to measure the density-viscosity of a given fluid is the circuit of the generator. The schema generator device, described the amplitude resonantly frequency, which is sensitive to the physical properties of the fluid, in which are immersed the crystal.

The second type of the resonator oscillations of the shear thickness, which can be useful for the practical implementation of the present invention, is disclosed in "Sensors and Actuators A44(1994)209-218 authors S. J. Martin, and others, the disclosure of which is included in this description by reference. This type of device uses the first sensor having a rough surface, and a second sensor having a smooth surface. Discovered that you can use such a device for the simultaneous determination and dissolution of the sediment mass, viscosity and density of the fluid. The use of smooth and rough surfaces that respond differently to the adhesion mass, helps to distinguish the deposition of mass and the viscosity and density of the fluid in contact with the piezoelectric crystal resonator oscillation shear thickness.

As described in U.S. patent No. 5201215, the mass of solids and/or physical properties of the fluid can be determined, when the mass, and fluid medium in contact with the same quartz crystal, by changing application of the electric field in the thickness Kwacha environment, measuring at least one resonant frequency of the quartz microbalance, simultaneous measurement of the full conductance at resonant frequencies and correlation of the resonance frequency and the magnitude of the full conductivity to obtain the mass density on the surface and works viscosity/density of the fluid. On the contrary, and as well as offers Granstaff, the oscillating electric field can be applied in thickness of the quartz microbalance, shaking frequency range that overlaps the at least one resonant frequency of the crystal by measuring the magnitude and phase of the full conductivity in the frequency range, correlating data full conductivity with frequency, and passing the data correlation full conductance/frequency equivalent model of the circuit, bringing into contact of the mass of solid and/or fluid from the crystal, and the solid mass is placed between the crystal and the fluid medium, repeating swing stage frequency range, which overlaps the resonant frequency, measuring the magnitude and phase of the full conductivity in the frequency range and correlating data full conductivity with frequency, and then throwing the data correlation full conductance/frequency equivalent model of the conductance/frequency.

Although Granstaff and others reveal that the layer of pulp may be metal alloys, salts, some stiff polymers or ice, and that these solids can be deposited on a quartz microbalance by evaporation, electroplating, coating, deposition, or by other chemical or thermodynamic reactions, Granstaff, etc. are not appreciated that the method can be effectively applied in the processing of hydrocarbons or water treatment, or that the device can be effectively used to control for the introduction of additives into the process in these areas.

The applicant has discovered, however, that a certain type quartz microbalance, essentially as described in the application Granstaff, can be used to overcome the disadvantages of the known devices using quartz microbalance, and can give accurate and instant data to control the supply of chemical products used for the control and modification of both aquatic and non-aqueous processes.

Therefore, a variant of implementation of the present invention provides a method of monitoring chemical additives in the processing of hydrocarbons and purification of water using devices resonate is to place accurate method of monitoring in real time for submission of chemical additives in the processing of hydrocarbons and water purification.

Another variant of the embodiment of the present invention provides an accurate method of monitoring in real time for filing the adjustment of status of chemical additives in the processing of hydrocarbons and water purification.

Additional embodiments of the present invention will be apparent hereinafter.

The invention

The primary method according to the present invention includes the use of the device of the resonator oscillations of the shear thickness, the installation of such a device where the surface of the quartz crystal may be in contact with the fluid medium, which in this case may be liquid or vapor (gas), dimension and weight, and works viscosity/density of the fluid, determining the status of the system and adding chemicals to handle or take such other corrective action as obtaining mass and works viscosity/density of the fluid. The device with the oscillations of the shear thickness can be mounted on the surface of the reservoir for such fluid, or may simply be omitted in the fluid. When the device is lowered into the fluid or temporarily, or permanently, should peregoy. The device of the resonator oscillations of the shear thickness is preferably mounted on the surface of the reservoir containing the fluid. Used the term "reservoir" means a pipeline, tank or any other device that contains the fluid.

The invention is applicable to the determination of the properties of water and non-aqueous systems. Among the principles used in the invention are the definition of scale, corrosion and biogarantie in aqueous systems, the determination of organic substances, deteriorating quality, and corrosion in hydrocarbon processes and the determination of the velocity stratification as emulsions of water in oil and oil emulsions, identification of characteristics of the fluid such as viscosity, density, percent solids, etc., the amount of sediment present in the tank or vessel, and the speed with which the formation of such deposition. As indicated, these are only some of applications of the invention in the field of water purification and processing of hydrocarbons.

Used the term "clean water" means preventing the formation of inorganic scale, corrosion, and biogarantie on surfaces in contact with the supplied water or technical is fouling, taking place in the water system. The term "water treatment" also includes the separation of solid particles from fluid or vapors, or liquids, or using chemical and/or physical means, and using the separation of oil from water, again using either chemical and/or physical means. Used the term "processing of hydrocarbons" means the transportation of crude oil by pipeline, rail, barge or tanker and refining this crude oil into useful products through various means, including the processes of desalination, distillation, cracking and other means to obtain marketable products, as well as additional processing such hydrocarbon products in the chemical industry, including the production of these valuable substances, as stiren, butadiene, isoprene, vinyl chloride, ethylene, propylene, Acrylonitrile, acrylic acid, alkylacrylate, and polymerization products formed from such substances. In practice the subject invention can be applied in any situation where you want to know the speed with which the formation of organic contamination on the surfaces of heat transfer equipment, pipelines, tanks for storage, etc., the Resonator with KOLEBANIYa, where you can expect organic impurities, inorganic scale, corrosion and microbiological fouling, or where a change in the characteristics of the fluid may indicate problems in processing, which can be adjusted by adding chemical products for special purposes. Similarly, the subject invention can be used to determine the speed with which it can be layered emulsion, or the state of emulsion in real time to allow the addition of a suitable substance for separation of the emulsion (or, conversely, emulsification of the desired product, emulsifier). Since the use of the present invention allows receiving real-time data, the control scale, contamination, microbial growth, etc., is done quickly and correctly achievable in an unprecedented way. The applicant is not known by any other method that can provide simultaneous instantly receive real-time data about the deposition of mass and the properties of the fluid for controlling the supply of chemical products for water treatment and/or chemical processing of hydrocarbons.

In one NWO is a seat on the surface of the tank, containing such fluid environment, and immediate serial or taking the steps to correct such condition, and the method includes the following stages:

A. put the device resonator to fluctuations in shear thickness in the reservoir and cause the quartz surface of the resonator oscillations of the shear thickness in contact with the fluid medium,

C. continuously excite the device resonator to fluctuations in shear thickness and measure the frequency shift and components of decaying voltage of the output signal of the resonator oscillations of the shear thickness,

C. continuously determine the state of the device surface of the resonator oscillations of the shear thickness on the basis of the frequency shift and components of decaying voltage, and then

D. continuously adjust the state specified on the device surface of the resonator oscillations of the shear thickness, through the actions of the group consisting of:

i. activating or deactivating the pump chemical products, supplying state-changing chemicals in the fluid,

ii. the increase in the flow of fluid from the system, or

iii. the mind is which are the output signals of the resonator oscillations of the shear thickness, can be used directly, it is often useful to convert these data into a mass component and the viscosity-density. As noted above, the device of the resonator oscillations of the shear thickness may be placed adjacent to the surface of the reservoir containing the fluid, or may be lowered into the tank in any place contained in the reservoir fluid is in contact with the surface of the quartz crystal device of the resonator oscillations of the shear thickness. Applied reservoir may be selected from the group consisting of installations for the processing of hydrocarbons, tanks for storage of hydrocarbons, pipelines or transport vessels such as barges, ships and railcars.

Moreover, although the device of the resonator oscillations of the shear thickness according to the invention can be placed in the system, it is also possible to place such a device in the system temporarily to determine whether to added chemical products, correcting the condition of the fluid.

Although the invention is useful for the correction condition on the surface in contact with the fluid medium, it can also be used for monitoring the status of Tecuci as consistency, viscosity, etc., In one of his examples in its broadest sense, the invention includes determining the status of the fluid in the process of obtaining a fluid medium, including the storage or transportation of the specified fluid, and simultaneously taking steps to correct such condition, and these steps include:

A. placed in a tank containing the specified fluid environment, the device of the resonator oscillations of the shear thickness, whereby the quartz surface of the resonator oscillations of the shear thickness is brought into contact with the fluid medium,

C. continuously excite the device resonator to fluctuations in shear thickness and measure the frequency shift and the components of decaying voltage of the output signal of the resonator oscillations of the shear thickness,

C. continuously determine the state of the device surface of the resonator oscillations of the shear thickness on the basis of the frequency shift and components of decaying voltage, and then

D. continuously adjust the state specified on the device surface of the resonator oscillations of the shear thickness, through the actions of the group consisting of:

i. aktiviranje in the fluid,

ii. the increase in the flow of fluid from the system, or

iii. reducing the flow of fluid from the system.

For another application of the invention, the invention in this application is running in the water purification system using the following steps:

A. introducing into the water, preferably on the surface of a tank containing water, the device of the resonator oscillations of the shear thickness, whereby the quartz surface of the resonator oscillations of the shear thickness is brought into contact with the fluid medium,

C. continuously excite the device resonator to fluctuations in shear thickness and measure the mass of the component and the viscosity-density of the output signal of the resonator oscillations of the shear thickness,

C. continuously determine the condition on the surface of the device resonator to fluctuations in shear thickness on the basis of mass and component viscosity, density, and then

D. continuously correct the condition defined on the surface of the device resonator, the oscillation of the shear thickness by the action of the group consisting of:

i. activating or deactivating the pump chemical produkuja environment of the system, or

iii. reducing the flow of fluid from the system.

While in the above description, the term "device of the resonator oscillations of the shear thickness" is used in the singular, it is often necessary to use more than one device resonator to fluctuations in shear thickness in a given system. As such, the singular term "resonator oscillation shear thickness" is used here to include one, two, or multiple devices of the resonator oscillations of the shear thickness. This allows more control over the system. The use of multiple devices of the resonator oscillations of the shear thickness is especially important when the device is used to determine the sediment in the tanker, the efficiency of separation of the emulsion, the level of foam in the tank, the level of each of the two or more different phases in the tank, etc.

The use of this invention allows to determine in real time the parameters that affect the water system. Using this method, the formation of scale, corrosion or biological contamination can be visually identified in the system much earlier than other measurement techniques can provide such Gee, determined much earlier than traditional methods, and corrective actions through the use of appropriate inhibitors scale formation or corrosion or microbiocidal can be started immediately to control the problem. By fast control system by using the methods according to the invention can achieve excellent control of industrial systems. Using device resonators with varying shear thickness in this way, can be made rigid control of water purification systems. The resonator oscillations of the shear thickness also works in real time, allowing you to avoid problems with the capture of chemical products on the analysis of the sample, which are composite (integrated over time) samples. This type of control does not indicate state violations when they occur.

In non-aqueous system, for example, an installation for the processing of hydrocarbons, the invention can in real time to determine the status of the contamination, corrosion and/or fouling on the surface of plants for the processing of hydrocarbons in contact with a hydrocarbon fluid medium (or liquid or gas the functions of this state. These steps include:

A. put the device resonator to fluctuations in shear thickness in the fluid contained in the plant for processing of hydrocarbons, whereby the quartz surface of the resonator oscillations of the shear thickness is brought into contact with hydrocarbons,

C. continuously excite the device resonator to fluctuations in shear thickness and measure the mass and component viscosity, density,

C. continuously determine the state of the device surface of the resonator oscillations of the shear thickness on the basis of mass and component viscosity, density, and then

D. continuously adjust the state specified on the device surface of the resonator oscillations of the shear thickness, by activate or deactivate the pump, which supplies state-changing chemicals in the plant for processing of hydrocarbons.

Again, because of the sensitivity of this method, pollution and the formation of scale can be determined at very low levels, and corrective actions can be taken immediately and, therefore, before the occurrence of major problems. As indicated above, although the device resonator Dow so, to the quartz crystal resonator with fluctuations of the shear thickness was in contact with the fluid medium, in the most broad sense of the invention it is only important that the surface of the quartz crystal device of the resonator oscillations of the shear thickness was in contact with the fluid medium, which need to be measured. When using the method according to the present invention, it should be expected that the main problems such as precipitation of asphaltenes on the surface of the heat transfer device at a refinery, can be spotted before they become serious or life-threatening, such as out-of-control exothermic polymerization in the storage tank monomers. Note that these are just examples of the use of the method according to the invention, and assistants for the processing of hydrocarbons in the production and refining of crude oil, cleaning and getting petrochemical products will easily see other areas, which can be used in the present invention. The equipment for processing of hydrocarbons, which may be applied a method according to the present invention, includes any equipment that processes crude oil or distillate to obtain fuel or neftech the p storage or reactor. Similarly, the invention is applicable to almost any facility for the processing of hydrocarbons, including installations for the processing of alkenes and alkynes (i.e., ethylene, propylene, styrene, Acrylonitrile, acrylic acid, alkylacrylate, vinyl chloride, butadiene and isoprene), as well as installation for further processing, which carry out further processing of alkenes and alkynes. Chemical additives that can be controlled include inhibitors of the formation of scale and corrosion inhibitors, antiparasites, Antiprotozoal, antiparasitary, etc. Should be understood that this invention is not limited to a specific type of chemical additive to any particular process.

The invention can also be used to determine the viscosity, density or state of the viscosity/temperature hydrocarbon fluid present in the tank, and im taking the steps for the correction or modification of this condition. The steps include:

A. put the device resonator to fluctuations in shear thickness in a tank containing such a hydrocarbon, whereby the quartz surface of the resonator oscillations shift Lebanese shear thickness and measure the mass and components viscosity, density,

C. continuously determine the state of the hydrocarbon fluid on the basis of mass and components viscosity, density, and then

D. continuously adjust the state of the hydrocarbon fluid through the activate or deactivate feed pump chemical products, feed changes the status of chemical products in the hydrocarbon fluid environment, are in the specified container.

This method is useful, for example, processing of diesel fuel or other fuel, which requires adding depressant additives to maintain adequate fluidity or other such additives, for example, improve the viscosity index, or other additives, which changes the property of the hydrocarbon fluid. Similarly, as in the water system, the invention can be useful for determining the presence and level of pricing in the process, and can be useful when introducing antiprotozoals in the manufacturing system.

The invention may also be useful when using rasseivatelei emulsion (or, conversely, emulsifiers in oil emulsions or emulsan water in the oil, such as those which are obtained by processing still remain the second way is usually two or more devices of the resonator oscillations of the shear thickness, according to the invention, placed at different levels in the tank containing the emulsion. The distinguished characteristics of the fluid, usually containing two or more immiscible liquids, can be obtained using resonators with varying shear thickness and accumulated data about the state of the emulsion at any particular level in such vessel or tank. Because of differing viscosity and density of water and oil and any intermediate inhomogeneous layer may be followed by separation of the emulsion, and can be added to the emulsion in the determination of the mass, viscosity and density made using resonators with varying shear thickness. The method of determining the state of a mixture of hydrocarbon/aqueous fluid and the flow of rasseivatelja emulsion for such a system usually includes the following stages:

A. placed in a vessel that stores or contains a mixture of hydrocarbon/aqueous fluid, the device of the resonator oscillations of the shear thickness, whereby the quartz surface of the resonator oscillations of the shear thickness is brought into contact with a mixture of hydrocarbon/aqueous fluid medium,

C. continuously excite usteristrasse determine the state of a mixture of hydrocarbon/aqueous fluid medium on the basis of mass and components viscosity, density, and then

D. continuously adjust the status of a mixture of hydrocarbons/water fluid through activate or deactivate feed pump chemical products, feed changes the status of chemical products in the treatment plant, containing a mixture of hydrocarbon/aqueous fluid medium.

Although this option may not be implemented in practice using only one of the resonator oscillations of the shear thickness, located in the tank at the level at which you want to measure what is present phase, it is often useful to apply two or more resonators with varying shear thickness, located on different levels of the tank or tanks to determine the state of the fluid at each of the measured levels. In the most preferred mode of practical implementation of this variant embodiment of the invention use at least two devices, one of which is preferably located at the level of the presence of the aqueous phase, and at least one of such devices is located at the level of determining the presence of hydrocarbons. The additional device can be used at the level of Gagliardo/water fluid medium, to be processed, usually contained in the vessel selected from the group consisting of reservoirs deemulsification crude oil heaters-cleaners crude oil, devices desalting of crude oil, columns cooling the ethylene furnace systems, generating liquefied pairs, tanks for storage of hydrocarbons, tanks for the transportation of hydrocarbons, sewage tanks, devices, wastewater treatment tanks for deposition, storage, and graceadelica the fluid after processing the metal. The use of more than one resonator to fluctuations in shear thickness provides the operator of the process of separation of the emulsion instant information about the real time status of the emulsion and the control flow in the emulsion correction state of demulsification or other chemical product. Used in the sense indicated above, the term "mixture" means an emulsion of water in oil, oil emulsion, emulsion anisotropic layers separated oil layers and separated by water layers, as well as dispersion of solid particles in liquids.

Although this method is described as suitable for the separation of emulsions, the way, of course, can be applied to obtain emulsions. Ispolzovanyi the emulsifying agent may be added to obtain an emulsion having the required characteristics.

As you can see, each of the described embodiments of the invention takes advantage of the resonator oscillations of the shear thickness. When using crystal resonator oscillation shear thickness to determine the number of available scale deteriorating quality substances and/or corrosion, the resonator oscillations of the shear thickness is set so that the affected side of the quartz was in direct contact with circulating in the fluid medium. When building such systems it is important to take into account the turbulence of the fluid caused by the presence of the resonator oscillations of the shear thickness. Accordingly, when measuring the contamination, fouling, corrosion or even the viscosity or other characteristics of the fluid, it is often beneficial to set shipped resonator with fluctuations of the shear thickness on the surface of the tank or pipe through which flows a fluid environment. When immersed placement in practice is not used, or when the crystal resonator oscillation shear thickness cannot be installed submerged on the surface of the tank or pipe through which fluid flows, the specialists easy to Opsa critical to the affected surface of the resonator oscillations of the shear thickness in contact with the measured fluid medium or fluid medium from which the deposited scale or dirt.

In another embodiment, the invention can be used portable resonator oscillation shear thickness. In its simplest form, a portable mount can be easily inserted in the fluid or in the free space of the tank, barrels or open container.

The surface of the quartz crystal resonator with fluctuations of the shear thickness according to the invention can be as small as necessary, or as big as possible to implement. Quartz microbalance of this type that you want to create cavities with the oscillations of the shear thickness, suitable from the point of view of practical implementation of the present invention, available in various sizes from many commercial sources. One of the features of the present invention is that the resonator oscillations of the shear thickness allows for quick and precise determination of the condition and measurement parameter to control the condition. The invention is applicable to a wide scatter of pressure to the quartz were equally compressed. When only one side of the crystal is exposed to high pressure, there may be distortion of the crystal, causing an inaccurate reading results. Similarly, the invention is useful for a wide range of temperatures varying from essentially below the freezing point up to the melting point of electrical connectors used to receive signals from a quartz crystal. As such, although the device is not directly suitable section of the pyrolysis, for example, ethylene furnaces, the device is suitable for use at the point of exit from the oven.

Among the many applications of the resonator oscillations shift to the thickness of such a device is used to control the addition of chemicals for special purposes, which are intended to improve or, on the other hand, to mitigate the condition, for example, activate or deactivate the pump containing microbicide, corrosion inhibitor, scale inhibitor, an inhibitor of pollution, etc. are Well-known ways to build circuits that control the pumps, using an output signal of the resonator oscillations of the shear thickness. Such schemes use the signal after determining through calibration level trebuemogo what that means. In addition to the actuation means of the pumping signal can be applied to open or close the purge valve in the cooling system or boiler, or to increase or decrease the flow of hydrocarbon fluid passing through the system, reducing or increasing residence time of the emulsion within the vessel, which is necessary for the separation of such emulsions, etc.,

During operation of the resonators with the oscillations of the shear thickness suitable for this invention is the schema generator to maintain a constant potential on the piezoelectric crystal (quartz crystal) to obtain stable oscillation. The output signal is measured and processed in accordance with the General principles explained in the aforementioned U.S. patent 5201215.

Although the current preferred mode of the invention is to use the calculated mass and the results of the viscosity-density, obtained by processing the original data generated by the device Granstaff, the output source data, the frequency shift and attenuation of the voltage obtained using the scheme described by Granstaff and in U.S. patent 5416448, Rato on the surface of the sensor, and can be applied directly without conversion to the values of physical characteristics. This method can be particularly useful when it is difficult to obtain exact values of the mass or properties of the fluid. In such applications the chemical additive can be controlled through the empirical observation of the frequency and/or voltage output.

These source data are also, of course, the measurement values of the components viscosity, density and mass of the fluid in contact with the piezoelectric device, and the invention encompasses the management of processes using a special chemical products, using either the original frequency shift and the data voltage, or components of the mass and viscosity-density, calculated from the original data.

Examples

Acrylonitrile usually recover from a gaseous stream resulting from the catalytic reactor, by extraction with water in the column, known as the absorber. Hydrogen cyanide and Acrylonitrile selectively extracted from the flowing stream, and the mixture is selected from the top after evaporation in the column recovery for submission to the column, where Acrylonitrile is separated as a pure component for FDI are removed by distillation in organoclay column, and most of the remaining water is sent back to the absorber in such a cyclic process of recovery. Efficient operation of the recovery process is limited by the presence of aggravating qualities of the substances present in the process, especially in the heat transfer equipment, such as reboiler, heat exchangers and distillation columns. This problem can be alleviated by adding a commercially available special chemical antiparasitary. Adding Antsiranana substance to the process with a dosage of 0.001-1000 ppm can significantly slow down the rate of pollution process and then increase the time of operation of the device, reducing the number of periodic cleaning of the equipment, and to improve the device performance. Ratio add antiparasites to devices of this type currently based on laboratory testing or empirical data on the number of days during which the device may be left in the process with a given dosage of antiparasites. In practice, the operating time of the heat exchanger is too short because of the presence of contamination, the dosage of antiparasites increases until, until you get acceptable is assitalia, as the dosage of antiparasites maximized for the worst possible condition and is not based on the actual state of pollution in the device. There is no way in situ, real time, in real-time to determine the optimal dosage of antiparasites.

In order to control the dosage of antiparasites, quartz sensor of the type described set is critical in the process of purification of Acrylonitrile. Typical places that can be installed resonators with waves shear thickness, are a stream of an aqueous solvent immediately before the heat exchanger. This sensor is positioned so that it protrudes into the flow of the water solvent. Crystal actuate the circuit on the outer wall of the pipeline. Generator and crystal connected by means of a sealed RF circuit, located on the outer side of the pipeline. The generator produces an output signal of specified frequency and amplitude. Changes in resonant frequency indicate changes in mass on the crystal surface and/or to modify the properties of the fluid. Changes in the amplitude reflect the weakening of the crystal. Measuring the damping of the crystal are particularly suitable ISM may have a high viscoelasticity. Viscoelastic deposition in Acrylonitrile process prevent the use of other sensors based on quartz crystal microbalance, which does not explain the influence of viscoelastic properties. Attenuation is also important to change properties of the fluid, since the resonant frequency is sensitive to each. Traditional quartz resonator sensors could not meet this requirement, because these devices are sensitive only to changes in the resonant frequency. Used in the invention, the sensor is suitable for process control, as the associated schema generation is sensitive to changes in resonance frequency and changes in the amplitude (fading voltage).

In the sensor, placed in the trunk of an aqueous solvent, an output signal of the generator is measured by the speed meter and voltmeter, and each of them connected to a personal computer. Other measurements include time and temperature. Using the output signal generator, a computer is used to calculate and plot the rate of accumulation of mass on the crystal surface. This speed is then determined prior to the introduction of antiparasites in the process, and the deposition rate in NSW is about control over time, when antiparasitary is introduced into the system. Dosage of antiparasites must then be adjusted up until the speed begins to change. This is evident from the testimony on the computer in the form of changes of the slope of a line, which is the result of plotting deposited mass from time to time. In the end, the dosage of antiparasites slowly run up until the slope of this line is zero (not defined deposition within a specified period of time) to obtain an optimized dosage of antiparasites. Optimized dosage set by measuring in real time better than chaotic variables, which can easily have an effect of other process variables. At any time during the test by increasing the deposition speed of antiparasites increase to offset the higher rate of contamination.

Alternatively, the placement of the resonator waves shear thickness in the flow of the aqueous solvent can be used a small rolling stream, taken from the recovery process of Acrylonitrile. In some cases, it can be expected that the total deposition of solid particles in the total volume of aqueous solvent is salivahanan small stream of water solvent is directed to a flow cell, containing the resonator wave shear thickness. The deposition of solid particles from a moving stream is proportional to the deposition of the total amount of aqueous solvent, provided that such process parameters as temperature and pressure are maintained at constant levels. To facilitate these conditions flow cell can be heated by means such as heating rods, band heater, water vapor or other conventional means. In addition, it may also be useful to add the regulator back pressure to the pipeline moving stream to maintain a constant pressure. In this case, the resonator wave shear thickness in the flow cell is connected to the circuit of the generator with the external side of the flow cell and tubing of a moving stream. The output signal generator is used, as described above, to calculate the deposition rate and optimizing the supply of antiparasites.

As obvious to the experts, the microprocessor can replace components such as a voltmeter and measure the frequency. The microprocessor can make the device more suitable for them and will allow the use of data recorders and desktop computer. In another possible embodiment, the computer is used for automatic control of the stroke of the pump, adding antiparasitary in Acrylonitrile process. The computer is programmed to adjust the stroke length of the piston to some extent when the proportional change in the rate of deposition of solid particles on the surface of the crystal. When the rate of pollution falls to zero, the computer must force the pump to maintain a constant length of stroke of the piston or decrease the stroke length of a few percent. Thus, the dosage of chemical antiparasites automatically optimized.

The resonator oscillations of the shear thickness can also be useful for monitoring the addition of Antsiranana to other processing operations hydrocarbons. As the next example this hypothetical example discloses the use of the resonator oscillations of the shear thickness to control add antiparasites to washing with caustic ethylene installation.

In the ethylene plant of the so-called acid gases such as carbon dioxide and hydrogen sulfide, are removed from the hydrocarbon mixture by flushing rakoobraznyh hydrocarbon solution of caustic soda. This is usually the wetlands due to polymerization with catalyst-based reactive aldehydes, similar to acetaldehyde. Pollution in the caustic tower and associated equipment can be controlled with the use of commercially available antiparasitary. In most cases there is no conventional way to determine the optimum dosage of antiparasites required to reduce contamination to acceptable levels, or eliminate pollution. In some cases, which may not be satisfactory, attempts were made to establish the dosage of antiparasites based on the amount of acetaldehyde, which is served in a caustic column. In one possible configuration, the resonator oscillations of the shear thickness can be installed in the fluid environment of the lower part of the column. The definition of solid particles in the residues from the bottom of the column indicates the amount of pollutants generated during the washing of the hydrocarbon gas. The response of the sensors can be used to set the optimal dosage of antiparasites caustic columns required to resolve the pollution in caustic column. Determination of small amounts of solid particles or their absence in the residues from the bottom of the column determine the optimal dosage of antiparasites.

During recovery of light oil products in the ethylene units, butadiene units, isoprene units, etc., distillation columns and associated equipment such as heat exchangers and reboiler, polluted thermal and/or oxidative polymerization of reactive olefins such as butadiene. Placing the device resonators with varying shear thickness suitable for the present invention, in the steam space below the selected plates, columns, can be used in tests to determine the formation of impurities in the vapor phase. Usually this definition is a very difficult problem up until the polymer pollutants, often referred to as "samobytnymi polymers", do not destroy the equipment in the column. "Samoobrona" polymers grow from the vapor phase on the metal surface in the column.

Resonators with varying shear thickness can be placed in the vapour space of the columns, such as primary fractionation columns, depropanizer, debutanizer and column purification of butadiene. Resonators with varying shear thickness is sensitive to the formation of a viscoelastic polymer in the vapor phase, which acadianas above. If detected the formation of impurities in the crystal, the dosage of antiparasites vapor phase may be adjusted accordingly. Thus, it can be determined the exact number of antiparasites required to control vapor phase.

Column recovery of hydrocarbons is also polluted in the liquid and gaseous phases. The placement of the resonator oscillations of the shear thickness described above, in the liquid residues from the bottom of the column can help to detect solid particles, which are deposited in the remains from the bottom of the column and associated reboiler. These sensors can be used to control the number of antiparasites, which is added to the residues from the bottom of the column and reboiler. These additives are usually different from those that add to control pollution vapor phase, although the contaminants are usually similar viscoelastic polymer, which is insoluble in the liquid hydrocarbon.

Sometimes the contaminant enters the column from another source. Consider adding pyrolysis gasoline in a primary fractionation column. In some cases, the spent caustic is washed pyrolysis gasoline to remove benzene from spent ka is lisnyy gasoline sometimes used as phlegmy primary fractionation column. During the washing of the spent caustic is formed alderny polymer through polymerization of phenylacetaldehyde with caustic catalyst and other reactive carbonyl particles in the pyrolysis gasoline. Any soluble resin formed in this process, comes in a primary fractionation column, where some part of the resin deposited on the equipment inside the primary fractionation column. The accumulation of resin in the primary fractionation column leads to contamination of the column. Found that pyrolysis gasoline from organicrich sections benzene contains up to 1 gram of resin in 100 ml of gasoline. Commercially available dispersants may be added to gasoline to facilitate control over the deposition of the resin in the primary fractionation column. Placing the device resonator to fluctuations in shear thickness according to the invention in the pipeline process that returns the phlegm in the column, can be used as an indicator of the amount of tar in pyrolysis gasoline the phlegm. Feedback from the sensor can be used to determine the appropriate dosage of antiparasites required to maintain the resin in dispergirovannom state in the column. Sensors are not Talikota pyrolysis gasoline due to higher or lower concentrations of soluble resin in a liquid.

As described above, the resonator oscillations of the shear thickness can be used to control the growth of biofilms or "soft" scale, which cannot be measured by using the previously known devices based on quartz microbalance. Applications for water systems that can be controlled with the use of the resonator oscillations of the shear thickness, include the manufacturing processes of pulp and paper, in which microbiological fouling is a problem, water cooling system, in which the growth of bacteria and algae can pose a significant problem, and some waste treatment systems. The invention can also provide an improved method for splitting the refinery oil-water emulsion, separating the oil phase from the aqueous phase and for other systems in which different density fluids can be detected using the devices, resonators with varying shear thickness. Since the device of the resonator oscillations of the shear thickness can simultaneously measure the deposition of mass and changes in liquid properties such as density and viscosity, in contrast to the previously known schemes, devices, specimen collection bicovariance time for microbial growth. The output signal of the resonator oscillations of the shear thickness is directly linked with the growth of biofilms and can be used to control the feed pump chemical products. Can be developed appropriate control algorithms that can guarantee that the rate of film growth will remain within acceptable limits. Without the use of devices of the resonator oscillations of the shear thickness is only available method of direct measurement using sampling for analysis. Taking samples for analysis, however, requires the collection of a composite sample over a period of time and does not report a violation of the system when they occur. The real-time control possible using resonators with varying shear thickness, will allow you to quickly manage these disorders by changing the dosage of chemical products for special purposes.

Similarly, in column cooling there is a simultaneous deposition of mineral scale and microbiological fouling. The ability to measure and to distinguish between these two modes of contamination will provide an opportunity to optimize the cleanup column cooling. Described resonators with varying shear thickness and those to whom the works of the viscosity-density. The difference between these two properties will allow to optimize the correct dosage of chemical compounds for treatment from scale, and for the treatment of biocides.

The possibility of rapid measurement of the viscosity of the sample allows real-time control for adding a viscosity modifier for suspensions. The viscosity modifier is added to the suspensions used in the processing of precious metals, to reduce energy consumption in pumping equipment. The method according to the present invention enables operational control of the addition of these chemical cleaning products, using the same sampling methods of control described above.

As an example, the resonator oscillations of the shear thickness mounted on the wall of the machine for the production of paper in contact with the paper composition. The resonator oscillations of the shear thickness tazrout in accordance with the reaction to the increase in the mass of biofilm on the surface of the quartz crystal. In the deposition of biofilms on the surface of a quartz crystal resonator with fluctuations of the shear thickness sends a signal indicating the growth of the film. This signal increase, and begin filing microbiocides p is nalivajut, when the mass deposition or decreases or remains constant. Similarly viscoelastic properties of biofilms can also be used to control fouling biofilm. Using either method, a machine for the production of paper remain essentially free from fouling. Due to the sensitivity of the resonator oscillations of the shear thickness of Microbiocide add speed required to reduce fouling and reduce overuse of chemical products. This leads to reduced consumption of chemical products.

The resonator oscillations of the shear thickness set on the internal wetted wall industrial column cooling. The resonator oscillations of the shear thickness tazrout to indicate the deposition of mass on its surface, and amplify the signal and serves to pump designed to supply commercially available industrial Microbiocide. The pump delivers the substance of the biocide in the column cooling. As soon as it is noticed microbiological fouling, indicated by a change in mass or viscoelastic properties of the sample, the crystal resonator oscillation shear thickness will send a signal that indicates fouling, including pump is Tania, supply of biocide stop. Using this system, a cleaner column cooling, and consume and unload a smaller amount of biocide over time.

The examples are not intended to cover all the various applications that can be used for sensors according to the invention. Experts can easily determine that in addition to measuring the speed of degradation of hydrocarbon systems and control for such a deterioration in the quality of the sensors can also be used for such diverse applications as determining the speed at which exfoliates the emulsion in abesolutely, and achieving operational control of the supply of rasseivatelja emulsion, the speed with which must be added Microbiocide to final products, and the speed at which chemical products for processing must be filed in the flow of hydrocarbons to maintain its fluidity and preventing deterioration of quality.

1. A way to quickly determine the presence of scale, corrosion and biological fouling occurring on the surface in contact with process water contained in the technical water system, and take steps to correct t is line, whereby the surface of the quartz device of the resonator oscillations of the shear thickness is brought into contact technical water) continuously excite the device resonator to fluctuations in shear thickness and measure the output signal of the resonator oscillations of the shear thickness as the mass and characteristics of the viscosity-density industrial water in contact with the device resonator to fluctuations in shear thickness; (C) continuously determine the condition of water located on the surface of the quartz device of the resonator oscillations of the shear thickness based on the mass and characteristics of the viscosity-density industrial water, and then D) continuously adjusting the condition of the water in contact with the surface of the quartz device of the resonator oscillations of the shear thickness by the action of the group consisting of: (i) activating or deactivating the pump chemical products, supplying state-changing chemicals in water, (ii) increase the flow of water from the system, or (iii) a decrease in the flow of water from the system.

2. The method according to p. 1, in which technical water system is a column of cooling.

3. The method according to p. 1, which IMO shear thickness is biofouling, and the feed pump chemical products adds Microbiocide or toxicant in water.

4. The method according to p. 1, in which technical water system is an industrial boiler.

5. The method according to p. 1, in which the presence of scale, corrosion and biological fouling in industrial water is controlled by the supply of chemicals that change the state of industrial water, selected from the group consisting of inhibitors of the formation of scale, and biocide.

6. The method according to p. 1, in which the surface of the quartz device of the resonator oscillations of the shear thickness is placed on the same level with the surface of technical water system, through which passes the water and the surface of the quartz device of the resonator oscillations of the shear thickness is in contact with the process water.

7. The method according to p. 1, in which the surface of the quartz device of the resonator oscillations of the shear thickness placed in technical water system temporarily.

8. A way to quickly determine the status of scale, corrosion and biological fouling occurring on the surface installations for the processing of hydrocarbons in contact with a hydrocarbon fluid medium, and predprinimaniya shear thickness in the fluid, contained in the plant for processing of hydrocarbons, whereby the surface of the quartz device of the resonator oscillations of the shear thickness is brought into contact with hydrocarbon; C) continuously excite the device resonator to fluctuations in shear thickness and measure the output signal of the resonator oscillations of the shear thickness as the mass and the characteristic viscosity-density hydrocarbon fluid in contact with the device resonator to fluctuations in shear thickness; (C) continuously determine the state of the hydrocarbon fluid in contact with the surface of the quartz crystal resonator oscillation shear thickness, based on the weight and characteristics of viscosity, density, and then (D) continuously adjusting the state of the hydrocarbon fluid in contact with the surface of the quartz crystal resonator oscillation shear thickness, by activation or deactivation of the pump, the feed adjustment state of chemical products in an installation for processing of hydrocarbons.

9. The method according to p. 8, in which the device for processing hydrocarbons may be the compressor, reboiler, heat exchanger, column purification, storage tank or reactor and pump podrabotka hydrocarbon selected from the group consisting of processing devices hydrocarbon producing alkenes and alkynes, and a feed pump chemical products delivers the one or more ingredients from the group consisting of inhibitors of contamination, corrosion inhibitors and Antiprotozoal.

11. The method according to p. 10, in which the device of the resonator oscillations of the shear thickness is placed on the surface of the device processing of hydrocarbons.

12. The device under item 8, in which the processing device of hydrocarbons selected from the group consisting of processing devices hydrocarbon producing stiren, acrylonitril, acrylic Kyoto, alkylacrylate, vinyl chloride, butadiene and isoprene.

13. The method according to p. 8, in which the device processing hydrocarbon processing crude oil and pump chemicals delivers the one or more chemicals, correction fluid hydrocarbon environment from the group consisting of inhibitors of contamination, corrosion inhibitors and antiprotozoals.

14. A way to quickly determine the status of the viscosity-density or state of the viscosity-temperature hydrocarbon fluid and taking the steps for correction or modification of this state containing phase, in which (A) help the surface of the quartz device of the resonator oscillations shift to the thickness of the lead in contact with hydrocarbon fluid medium, C) continuously excite the resonator oscillations of the shear thickness and measure the output signal of the resonator oscillations of the shear thickness as the mass and the characteristic viscosity-density hydrocarbon fluid, (C) continuously determine the state of the hydrocarbon fluid in contact with the surface of the quartz crystal resonator oscillation shear thickness based on the mass and characteristics of viscosity, density, and then D) continuously adjusting the state of the hydrocarbon fluid through the activate or deactivate feed pump chemical products, feed changes the status of chemical products in the hydrocarbon fluid environment.

15. The method according to p. 14, in which the hydrocarbon fluid contained in the reservoir is selected from the group consisting of a device for the processing of hydrocarbons, tank for the storage of hydrocarbons, pipeline or reservoir for transportation.

16. The method according to p. 15, in which the device of the resonator oscillations of the shear thickness is placed in a tank containing such hydrocarbon fluid environment temporarily.

17. A way to quickly determine the status of a mixture of hydrocarbon/aqueous fluid, stereodecoder A) is placed in a mixture of hydrocarbons/water fluid medium, at least one device resonator to fluctuations in shear thickness, whereby the surface of the quartz device of the resonator oscillations shift to the thickness of the lead in contact with the mixture of the hydrocarbon/aqueous fluid medium) continuously excite the device resonator to fluctuations in shear thickness and measure the output signal of the resonator oscillations of the shear thickness as the mass and the characteristic viscosity-density mixture of hydrocarbon/aqueous fluid, (C) continuously determine the state of a mixture of hydrocarbon/aqueous fluid based on the weight and characteristics of the viscosity-density of the above characteristics, and then D) continuously adjust the status of a mixture of hydrocarbons/water fluid through activate or deactivate feed pump chemical products, feed correcting the state of the chemicals in the mixture of the hydrocarbon/aqueous fluid medium.

18. The method according to p. 17, in which the mixture of hydrocarbon/aqueous fluid contained in the reservoir is chosen from the group consisting of a tank of deemulsification crude oil heaters - cleaners crude oil, devices desalting of crude oil, columns cooling ethylenemethacrylic hydrocarbons, the sewage tanks, devices, wastewater treatment tanks for deposition, storage, and graceadelica the fluid after processing the metal.

19. The method according to p. 18, in which the resonator oscillations of the shear thickness is placed on the surface of the tank so that the surface of the quartz device resonator in contact with contained in the tank mixture of hydrocarbon/aqueous fluid medium.

20. The method according to p. 18, wherein the surface of the quartz device of the resonator oscillations of the shear thickness is placed in a mixture of hydrocarbon/aqueous fluid temporarily.

21. The method according to p. 17, which use two or more devices of the resonator oscillations of the shear thickness, with one of the resonators are placed on the same level to determine the presence of the aqueous phase, and the other resonator is placed on a different level to determine the presence of hydrocarbons.



 

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3 cl, 1 dwg, 3 tbl, 3 ex

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