Method to control the process of production of polyethers and demulsifying agents on their base

FIELD: chemical industry; control over processes of production of polyethers and demulsifying agents on their basis.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the methods of control over the chemical-technological processes of production of polyethers and demulsifying agents on their basis. The method of control over process of production of the alkaline polyethers and demulsifying agents is conducted in the mixers and in the reactor-etherificator at realization of reaction of the oxypropropylation and oxyethylation with utilization of the allocated zones of regulation and contours of circulation of the reaction mixture. Conduct corrective actions of control over the steam and a condensate consumption moisture and at that additionally install a can with a bubbler for a polyether and a detector of methanol consumption, a reactants stirring device, sensor units of consumptions, measuring tools and other equipment. For production of demulsifying agents from polyethers use cans with stirring devices with measurers and batchers components, screens for removal salts and the mechanical impurities, connected by corresponding pipelines with formation of contours of circulation of the reaction mixture equipped by means of measuring and control. The technical result is formation of the interrelated process control of production of polyethers and demulsifying agents. The invention allows to reduce power inputs and to expand the assortment of the produced products.

EFFECT: the invention allows to form the interrelated process control of production of polyethers and demulsifying agents, to reduce power inputs and to expand the assortment of the produced products.

3 cl, 2 ex, 1 dwg

 

The invention relates to the production of polyethers and demulsifiers based on them and can be used in the chemical industry for process control in the advanced range of products based on polyesters.

A known method of controlling the polymerization process of polyethers in reactors polymerization periodic type by measuring temperature, pressure, reaction mass and stabilize them in the reactor cooling water to bypass the heat exchanger. On the partial vapour pressure of ethylene oxide change the flow of ethylene oxide and cooling water while maintaining the temperature in the reactor. (U.S. Pat. Of the Russian Federation No. 2046809, 08 With 65/08, 1995)

The disadvantage of this method of control is low, the accuracy of controlling the partial pressure due to the drift of the measurement parameters on which it is defined and limited scope, for example, cannot be used to obtain alkaline polyesters.

Closest to the proposed invention is a method of controlling the process of obtaining polyether held mixers, reactor-etherification periodic operation, the heat exchanger and the separator by stabilizing the costs of propylene oxide, ethylene oxide, the temperature of the reaction mass, flow measurement Faure is alimera, pressure and level in etherification. When running consistently use zone regulation temperature reaction oxypropylation and oksietilirovannye with the formation of loops of circulation of the reaction mixture. Depending on the set temperature reactions adjust the steam supply and condensate. (U.S. Pat. Of the Russian Federation No. 2141977, 08 G 65/06, G 05 D 27/00, 1999)

The disadvantage of this invention is inflated energy consumption (resetting the secondary pair), and limited scope, since it cannot be used to obtain neutral polyesters and demulsifiers based on them.

The task of the invention is to improve the efficiency and expand the scope of production of polyesters and demulsifiers based on them.

This object is achieved in that the known method of controlling the process of obtaining polyethers and demulsifiers based on them, held mixers, reactor-etherification periodic operation, the heat exchanger and the separator by stabilizing the costs of propylene oxide, ethylene oxide, the temperature of the reaction mass, measuring the flow of prepolymer, pressure and level in etherification, job control zones, the reaction temperature oxypropylation and oksietilirovannye correction control actions based on steam flow and to the of densata, further comprises a tank with a bubbler for polyester and flow sensor methanol capacity with a stirrer reagents for producing neutral demulsifier with dispensers Agidol and aspillaga and flow of demineralized water tanks to supply phosphoric acid and bentonite, filter press automatic chamber, rotary film evaporator, moisture, proceedings of the mixture to neutral demulsifier, filter press frame and the tank with a bubbler for the neutral demulsifier and a flow sensor methanol; ask the ratio of polyester:methanol upon receiving alkaline demulsifier; specify the ratio of polyester:demineralised water:phosphoric acid:bentonite:Agidol: astillo upon receiving the mixture to neutral demulsifier; set the ratio of the mixture to neutral demulsifier:methanol upon receiving a neutral demulsifier and adjust accordingly the cost of methanol in obtaining alkaline and neutral demulsifier. In addition, the ratio of polyester:methanol upon receiving the alkaline and neutral demulsifier is 90:70-10:30 wt.%, and the production capacity of the plant to polyester and emulsion breakers up to 4000 tons /year.

A set of additional devices and new management techniques in combination with known gives the production p is liferov and demulsifiers new properties, allowing to judge that the proposed solution meets the criteria of the invention.

The essence of the invention illustrated by the drawing, which shows a schematic diagram of a control process of obtaining polyethers and demulsifiers under conditions of industrial production.

The scheme includes apparatus 1-18, as well as sensors and valves 19-37. Propylene oxide (and then ethylene oxide) served in the mixers 1, 2, and later in etherification 3, which also serves a prepolymer derived from an alkaline catalyst, such as an intermediate product to obtain polyesters. For heating the reaction mass in the coils of mixers 1, 2 and etherification 3 serves pairs of high and low pressure valves on the scheme conditionally not shown). Then the reaction mass pump (turbo pump) 4 is directed into the heat exchanger 5, where the reaction heat is removed by the condensate, which is then sent to the separator 6 for catching drops and secondary steam is used to control the reaction oksietilirovannye. Then the reaction mass is sent to the mixers 1, 2, thus, a primary circuit circulation of the mixture through the apparatus 1-2-3-4-5-1-2 and additional circuit through the apparatus 3-4-5-3" if the reaction oxypropylation and oksietilirovannye. Obtained on the basis of selecing the catalyst for polyester is directed to a container 7 with a bubbler for polyester and forth to get alkaline and neutral demulsifiers. Upon receipt alkaline demulsifier in polyester add methanol. Upon receipt of a neutral demulsifier polyester pump 8 is directed to a container 9 with a stirrer to obtain a neutral demulsifier, which also served demineralized water and the individual components: bentonite, Agidol and astillo and from the measuring device 10 phosphoric acid. The resulting reaction mass pump 11 is directed into the container 7 and circulate through the apparatus, forming a circulation loop "11-7-8-9-11 for a specified time. After circulation of the reaction mass pump 8 (separate output) is sent to a filter press automatic chamber 12 to remove salts and then the mixture was fed to a rotary film evaporator, moisture 13, which, after removal of water is directed through the collector of the mixture to neutral demulsifier 14 to a filter press frame 16 to permanently remove salts and impurities and then into the container 17 with a bubbler for the neutral demulsifier. When cooking neutral demulsifier into the container 17 serves methanol and circulate the mixture by the pump 18 for circulating path 18-17-18 for a specified time. After additional mixing of the nitrogen supplied to the bubbler tank 17, a neutral demulsifier sent to the finished goods warehouse. Control system% is Scam includes: flow sensors 19 prepolymer, 20 propylene oxide, 21 ethylene oxide, the valve 22 supply of reagents; sensors 23 temperature 24 pressure and level 25 in etherification 3; valve 26 in an extra line of circulation of the mixture 3-4-5-3"; a valve 27 to supply steam to the turbine pump 4. The sensor 28, the temperature of the reaction mass, the valve 29 in the flow of condensate in the heat exchanger 5, the sensor 30, the temperature of the reaction mass, the valve 31 on the output line of the secondary steam from the separator 6. In addition, the control system includes: a flow sensor 32 of methanol in the tank 7, the dispenser 33 Agidol, dispenser 34 aspillaga, dipstick 35 bentonite, as well as flow sensors 36 demineralized water supplied into the tank 9 and methanol 37. When the control process uses the computer (conditionally on the diagram not shown).

The study of the production of the polyesters obtained using alkaline catalysts and demulsifiers based on them for dehydration and desalting of crude oil, showed that to improve the quality and efficiency of the products you need to make vzaimosvyazei management processes and, if neudovletvoriteleny indicators emulsifiers due to perturbations introduced in the process, you can adjust operational parameters at the stage of carrying out reactions oxoprolinuria and oksietilirovannye without stopping the apparatus, resulting in increased productivity and what allows to save energy, associated with start-up and shutdown.

The management process is as follows:

according to the sensor 19 serves a specified number of the prepolymer in etherification 3 and according to the information of the sensor 20 through the mixers 1, 2 also serves propylene oxide for the reaction of the oxypropylation; heated reaction mass of steam of high and low pressure lines, a pair of conventionally not shown);

- circulate through the apparatus by the pump 4, the reaction mass at the main circulation line 1-2-3-4-5-1-2" and more "3-4-5-3";

according to the sensor 30 determines the set temperature of the reaction mass and when it disables the secondary line circulation "3-4-5-3" effect on the valve 26;

according to the sensor 23 set the desired temperature of the oxypropylation reaction (from a given area of regulation, which adjust depending on the type of emulsifier) impact on the valve 29 when the flow of condensate in the heat exchanger 5, and when the desired conversion of propylene oxide (defined by the laboratory) stop the flow effect on the valve 22;

- information sensor 21 through the mixers 1, 2 served in etherification 3 ethylene oxide for the reaction of oksietilirovannye;

according to the sensor 28 set the desired temperature, R is the promotion of oksietilirovannye (from a given area of regulation, which is correct depending on the type of emulsifier) impact on the valve 31 in the selection of secondary steam from the separator 6;

- circulate through the apparatus by the pump 4, the reaction mass at the main circulation line 1-2-3-4-5-1-2" and when the desired conversion of ethylene oxide stop the flow effect on the valve 22;

according to the sensor 24 monitors pressure on sensor 25 level in etherification 3 and when the deviation from the setpoint is affected respectively by the valves 22 and 25.

The obtained polyester alkaline oil (PSN) pump 4 is directed into the container 7 with a bubbler to store and retrieve demulsifiers.

To obtain the demulsifier alkaline oil (DSN) specifies the ratio of the polyester-methanol", available on information sensor 32 methanol in the tank 7 and a nitrogen bubbler (line feed nitrogen conventionally not shown), stirred the mixture for a specified time, and the resulting product is alkaline demulsifier shipped to the warehouse of the pump 8 (on separate lines).

Obtaining polyester neutral oil (PNN) is as follows:

- polyester from the tank 7 (after holding for a specified time) of the pump 8 serves in the capacity of 9 with a stirrer reagents and for a given ratio of polyester:demineralised water:phosphoric Ki the lot:bentonite:Agidol:astillo served there components: according to information from sensor 36 demineralized water, from the measuring device 10 phosphoric acid, from the measuring device 35 bentonite and from dispensers 33, 34 Agidol and astillo;

- the resulting reaction mass is circulated through the apparatus by the pump 8 and 11 on the circuit "11-7-8-9-11 for a specified time;

after circulation of the reaction mass pump 8 serves to filter press chamber 12 to remove salts and then on a rotary film evaporator moisture and digest the mixture for neutral demulsifier 14;

after removal of the water mixture to neutral demulsifier pump 15 is sent to a filter press frame 16 to remove residual salts, particulate matter and then purified mixture is sent into the tank 17 with a bubbler for the neutral demulsifier.

Getting oil demulsifier neutral (DN) is as follows.

for a given ratio of the mixture to neutral demulsifier - methanol serves information on sensor 37 methanol. The resulting mass is circulated by the pump 18 through the tank 17 through the circuit "18-17-18 for a specified time and additionally stirred by feeding nitrogen into the bubbler tank 17. Received neutral demulsifier pump 18 shipped to the warehouse of finished products.

Thus, carrying out vzaimosvyazei management process of obtaining polyethers and demulsifiers, we have to reduce Energostal the t by reducing the number of start-up and shutdown of units of production. Getting alkaline and neutral polyesters based on demulsifiers, expanding the range of manufactured products enterprise, which allows to take into account the aspects of implementation of the required products and ultimately increase production efficiency as a whole.

Experimental verification of a control method carried out in an industrial installation in the 4th quarter of 2003 in OOO "Kama petrochemical company" , Nizhnekamsk has shown its effectiveness.

Below are examples of usage control method upon receipt of polyesters and demulsifiers.

Example 1

Getting alkaline polyester and demulsifier.

According to information from sensor 19 is served in etherification 3 the prepolymer in the amount of 1000 kg and according to the information of the sensor 20 there through the mixers 1, 2 serves propylene oxide in the amount of 9000 kg for the reaction of the oxypropylation (heated mixture of steam at 0.2 MPa and 1.6 MPa). Produce circulation of the reaction mixture by the pump 4 through the main line circulation "1-2-3-4-5-1-2" and more "3-4-5-3" (when you open the valve 26 during the heating of the mixture).

Control according to the sensor 28, the temperature of the reaction mixture and upon reaching 148°With switchable additional line circulation "3-4-5-3" effect on the valve 26.

Set according to the sensor 23 specified temperature reaction oxypropylation 150°who is esteem the valve 29 when the flow of condensate in the heat exchanger 5. Upon reaching the conversion of propylene oxide 93% closing valve 22 for the supply of propylene oxide.

According to information sensor 21 serves to etherification 3 through mixers 1,2 ethylene oxide in the amount of 4000 kg for the reaction of oksietilirovannye (valve 22 is open) and according to the information of the sensor 28 set the desired temperature of reaction oksietilirovannye 156°With effect on the valve 31 in the selection of the secondary pair. Circulating reaction mass on the main line circulation "1-2-3-4-5-1-2" and achieve the conversion of ethylene oxide 93% close the valve 22.

According to information from sensors 25 and 24 define a level equal to 3.2 m3and pressure, equal to 0.56 MPa. These parameters are within predetermined limits, so the impact on the valve 27 and 22 are not produced. The obtained alkaline polyester (PSN) 13090 kg directed into the container 7. Polyester corresponds to THE 2226-03-57266723-2003. Further, the polyester used in obtaining alkaline demulsifier (DSN). The specified ratio of the polyester-methanol" - 1:0.15 in. According to information from the flow sensor 32 serves in the capacity of 7 methanol amount of 1850 kg, stir the mixture by feeding nitrogen into the bubbler tank 7 to 2 m3/h and the number 14940 kg are sent to the warehouse.

Example 2

Getting neutral polyester and demulsifier

Polyester (obtained at the reaction temperature oxypropylation 154°and reactions about what siciliane 158° With analogously to example 1) in the amount of 15000 kg served from the container 7 by pump 8 into the tank 9, where for a given ratio of polyester:demineralised water:phosphoric acid:bentonite:Agidol:astillo"equal 1:6,6:0,63:0,33:0,33:0,0043 Rel. units are served according to the sensor 36 1000 kg of demineralized water, from the measuring device 10 phosphoric acid in the amount of 95 kg, from the measuring device 35 bentonite in the amount of 50 kg, the dosing device 33 Agidol in the amount of 50 kg and the dosing device 34 astillo of 7 kg Circulate (at a temperature of 110° (C) through the apparatus by the pump 8 and 11 the resulting reaction mass in circuit "11-7-8-9-11" within 6 hours

After circulation directed reaction mass on the filter press 12, where the removed salt up to 30 kg, and the mixture is then directed to a rotary film evaporator, moisture 13, which removed up to 1000 kg of water (under vacuum). Dehydrated mixture is directed into the collector 14 and the pump 15 to a filter press 16, where remove mechanical impurities and residues of salts to 17 kg Then neutral polyester (PNN) use for neutral demulsifier (DNN).

For a given ratio of the mixture to neutral demulsifier - methanol", equal to 1:0,16, served according to the sensor 37 in the capacity of 17 methanol in the amount of 2400 kg of the resulting reaction mass circulating pump 18 through the tank 17 through the circuit "18-17-18" for 10 hours and after will complement the high mixing feed in the bubbler tank 17 of nitrogen up to 2 m 3/h guided neutral demulsifier in the number 17300 kg to the warehouse of finished products.

Thus, the method allows to obtain the installation alkaline polyesters based on alkaline and neutral demulsifiers used in the petroleum refining and related regulatory requirements.

The implementation of the method of control is scheduled for Q1 2004 Kamsky petrochemical company", Nizhnekamsk. The economic effect from the introduction of up to 2 million rubles/year.

1. The process control method of obtaining polyethers and demulsifiers based on them, held mixers, reactor-etherification periodic operation, the heat exchanger and the separator by stabilizing the costs of propylene oxide, ethylene oxide, the temperature of the reaction mass, measuring the flow of prepolymer, pressure and level in etherification, job control zones, the reaction temperature oxypropylation and oksietilirovannye correction control impacts on the consumption of steam and condensate, characterized in that it further comprises a container with a bubbler for polyester and flow sensor methanol capacity with a stirrer reagents for producing neutral demulsifier with dispensers Agidol and aspillaga and flow sensor desalted water tanks to supply phosphorus is islote and bentonite, filter press automatic chamber, rotary film evaporator, moisture, proceedings of the mixture to neutral demulsifier, filter press frame and the tank with a bubbler for the neutral demulsifier and a flow sensor methanol, ask the ratio of the polyester-methanol upon receiving alkaline demulsifier; set the ratio of the polyester-demineralized water: phosphoric acid: bentonite: Agidol: astillo upon receiving the mixture to neutral demulsifier; set the ratio of the mixture to neutral demulsifier-methanol upon receiving a neutral demulsifier and adjust accordingly the cost of methanol in obtaining alkaline and neutral demulsifiers.

2. The method according to claim 1, characterized in that the ratio of polyester-methanol" upon receipt of alkaline and neutral emulsion is 90:70-10:30 wt.%.

3. The method according to claims 1 and 2, characterized in that the performance polyesters and emulsion breakers up to 4000 tons/year.



 

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