The process control method of obtaining caprolactam by reaction rearrangement cyclohexasiloxane

 

(57) Abstract:

The inventive regulate the total flow cyclohexasiloxane served in both reactors, the ratio of total consumption cyclohexasiloxane served in both reactors, and oleum supplied to the first reactor, the change of the flow of the latter. Regulate the ratio of costs cyclohexasiloxane served in both reactors, the change of the flow cyclohexasiloxane in the first reactor, the temperature of the solution in both reactors. Measure the moisture content in cyclohexanehexol. Measure the acidity of the solution in the second reactor. Adjust the flow of oleum in the first reactor, depending on the moisture content in cyclohexanehexol. Regulate the flow cyclohexasiloxane in the first reactor with the correction to the total consumption of cyclohexasiloxane served in both reactors, the moisture content in cyclohexanehexol and acidity of the solution in the second reactor. The temperature of the solution in the second reactor regulate with correction for General consumption cyclohexasiloxane served in both the reactor and the pH of the solution in the second reactor. 3 Il., table 1.

The invention relates to methods for process control, in particular about the procedure of obtaining caprolactam, includes stage rearrangement cyclohexasiloxane [1] the Optimal process of rearrangement is fast hashing cyclohexasiloxane with oleum with continuous removal of the heat, stabilization of the temperature regime and a given ratio of feed cyclohexasiloxane and oleum.

The disadvantage of the high specific consumption of oleum. This is because the control process is carried out only on the temperature and acidity of the reaction solution. Due to the fact that the heat removal carried out by cooling in heat exchangers of the reaction solution at the outlet of the heat exchanger, the viscosity of the reaction solution by lowering the temperature increases significantly and to reduce the flow of oleum carried out with an excess compared with the stoichiometric quantity.

There is a method of automatic control of a process for obtaining caprolactam, including the state of the rearrangement cyclohexasiloxane, by regulating the acidity of the rearranged product of the change in the flow rate of oleum, according to which regulate the content of sulfuric anhydride in the rearranged product by changing the supply of water in the oleum [2] the Application is of Idrija in the rearranged product.

However, the lack of high-precision and high-speed devices for the measurement in the rearranged product of free sulfuric anhydride, as well as the inadmissibility of leakage of moisture in the rearranged product, the content of free sulfuric anhydride in the rearranged product support at a sufficiently high level, which also leads to waste of oleum.

The closest to the technical complexity and the achieved result is a method for automatic process control of the rearrangement of the oxime in the lactam by stabilizing the concentration of sulfuric acid in the reaction mass change rate of the oleum and the stabilization of the concentration of sulfuric anhydride by changing the supply of water for dilution of oleum, according to which the supply of water to dilute oleum is performed with the correction for the moisture content of the oxime and the concentration of oleum [3] due to operational humidity measurement coming cyclohexasiloxane and concentration of oleum reduced content of free sulfuric anhydride in the rearranged product and, as a consequence, specific consumption of oleum.

However, the known method of control can significantly reduce the specific consumption of oleum at its abolition optimal temperature and load modes of the reactor when the load changes the installation. Non-optimal mode selection leads to uneven heat load reactors. The temperature of the reaction solution in the second reactor may be significantly higher than the temperature in the first reactor, and the achieved advantages (reduction of pitch, increase the yield of caprolactam and reduction of specific consumption of oleum) application of two-stage scheme will be negated due to thermal effects in the second reactor.

The purpose of the invention, the reduction of specific consumption of oleum.

This objective is achieved in that the process control method of obtaining caprolactam by reaction rearrangement cyclohexasiloxane, including the measurement of total consumption cyclohexasiloxane and humidity measurement and regulation of temperature, measurement of the acidity of the reaction solution and the flow control oleum depending on flow cyclohexasiloxane and acidity of the reaction solution according to the invention regrouping cyclohexasiloxane in caprolactam is carried out in two series-connected reactors with circulating heat exchangers, determine the relative load facility cyclohexanehexol and the acidity of the solution in the second reacto and installation cyclohexanehexol and the content of moisture, regulate the amount cyclohexasiloxane in the first reactor, depending on the total consumption cyclohexasiloxane served in both reactors, the moisture content in cyclohexanehexol and acidity of the solution in the second reactor. The temperature of the solution in the second reactor is adjusted depending on the relative load setup cyclohexanehexol and pH in the second reactor.

The claimed method allows to maintain optimum thermal conditions in the reactors without offset temperature. Achieved minimal thermal effect on organic products and, as a consequence, the minimum loss and maximum yield of caprolactam, which allows to reduce the specific consumption of oleum in terms of ton of caprolactam.

In Fig. 1 shows graphs of the variation of the viscosity of the reaction solution depending on the temperature and acidity, expressed in molar ratio of sulfuric acid (in terms monohydrate):oxime; Fig.2 the dependence of the minimum possible temperature of the circulating reaction solution depending on its acidity for maximum permissible viscosity 50 JV of Fig.3 schematic diagram of the proposed control method.

The dependence of the minimum possible temperature of the circulating reaction solution (Fig.2) from its acidity for maximum permissible humidity of 50 JV is an almost straight line in the field of molar relationship sulfuric acid:the oxime lying within 1.4-1,65 (characteristic of the second reactor), and can be expressed by the formula T 78,3 x Hm + 217,6, where M acidity (molar ratio of sulfuric acid:the reaction), the reaction solution.

It is known that the reduction of the load on installation allows for increasing the ratio of circulation to reduce the acidity of the reaction solution with maintaining the quality of mixing, i.e., the load reduction is equivalent to increasing the acidity of the reaction solution. In the working range of pH Meters 1,4-1,65 amaximal is a straight line M 1,1 + 0,5 G/Gm, where G and Gm load on the installation, the current and maximum, respectively.

Thus, at the working pH of 1.65 at 100% load correction factor = 1,65/(1,1 + to +0.5 G/Gm) and the acidity of the reaction solution will allow to reduce the consumption of oleum while reducing the load on the installation. The calculated value of TRasch.the temperature of the stream exiting the heat exchanger of the second reactor will be:

TRasch.to 78.3 M + 217,6 or

TRasch217,6 258,4 M/(2,2 + G/Gm).

If the temperature T1the stream exiting the heat exchanger of the first stage, set T180aboutC, and the temperature difference at the heat exchanger T1then the temperature of the reaction solution flowing in the heat exchanger 80 + T1.

Similarly, the temperature of the reaction solution flowing in the heat exchanger of the second reactor under the condition that the temperature of the outgoing stream T2TRaschwill be TRasch+ T2.

To reduce the overall viscosity of the reaction solutions and maintain minimal thermal impact on organic products is necessary to maintain the condition of equality of the maximum temperatures in contach the first and second reactors depends on the amount fed to each reactor cyclohexasiloxane and humidity. With the share = 0,65-0,85 feed cyclohexasiloxane in the first reactor, 100% humidity (humidity cyclohexasiloxane can be measured by the analyzer installed on the flow, or be determined by the laboratory for industries characterized by relatively stable moisture content in cyclohexanehexol), and given that the enthalpy of the reaction rearrangement r1496 kcal/kg oxime, and the dissolving of sulfuric anhydride r21128 kcal/kg of water, the heat exchanger of the first reactor will be

Q1= G[(1-)r1+)r2] and in the heat exchanger of the second reactor, respectively, Q2(1 ) Q1.

The temperature difference in the heat exchangers of the first and second reactors, respectively T1Q1/(cG1and T2Q2/(c G2, where to 0.35 kcal/kg heat capacity of the reaction solution; G1, G2the volume of the circulation paths, respectively, the first and second reactors.

Thus, the minimum temperature effects will be:

80+{G[(1-)r1+r2]/(cG)1TRasch+(1-)G[(1-)r1+r2] /(cG2).

Transform the last equation leads to the form:

G A (B + C) G A C + D, where A (1 ) r1is hexanolactone in the first reactor becomes:

G (G A (C + D)/[A (B + C)]

To install with the same circulation contours (G1G2B C, and the equation takes the form G (GAC + D)/(2AC).

The scheme of realization of the proposed method (Fig.3) consists of reactors 1 and 2, respectively, the first and second stages, equipped with circulation pumps 3 and 4 and the heat exchangers 5 and 6 with bypass lines 7 and 8. The circulation loop reactor 1 is equipped with a three-way valve 9 and the sensor 10. The circulation loop reactor 2 has a three-way valve 11 and the sensor 12. The reactor 2 is equipped with a sensor 13 of the acidity of the reaction solution. Supply line installation (in both reactors) cyclohexasiloxane equipped with a flow meter 14 and a control valve 15. Supply line cyclohexasiloxane in the first reactor is equipped with a control valve 16. Supply line of oleum to install an adjustable valve 17. The scheme also includes a block 18 of correlation, functional blocks 19,20,21,22 and 23, a controller 24, the blocks 25,26 and 27 multiplication, the adder 28 and block 29 division.

The method is as follows.

Cyclohexanone serves to install and measure its flow by the flow meter 14, the output signal G which is representing Sobornosti. Block 18 ratio based on the signal G current consumption cyclohexasiloxane and setpoint Gm maximum possible feed on the plant generates a signal G/Gm a relative load of the installation.

Functional block 19 calculates the signal L control of the regulating valve 17 filing for the installation of oleum depending on the plant load, feed her cyclohexasiloxane and humidity, maintaining the optimum molar ratio of sulfuric acid:the oxime. Due to the fact that the molar ratio corresponds to the formula M L1,045113/[G(1 )98] where 1,045 conversion factor of 20% oleum in the monohydrate;

the relative moisture content in cyclohexanehexol;

113,98 molecular weight, respectively cyclohexasiloxane and sulfuric acid, and given that M 1,1 + 0,5 G/Gm, flow L oleum will be:

L 0,41 G(1 )(2,2 + G/Gm).

Oleum in the required amount through the control valve 17 into the reactor 1 via the suction line of the pump 3. Mixed with oleum circulating the reaction solution through the heat exchanger 5, the bypass line 7 and the three way valve 9 into the reactor 1. The amount of solution passed through the bypass line 7, is determined by the desired temperature (80about(C) entering R and the temperature of the reaction solution, arriving in reactor 1, above 80aboutWith the three way valve 9 reduces its flow section from the side of the bypass line 7 and extends from the side of the heat exchanger 5. Thus the flow through the bypass line 7 is reduced, and through the heat exchanger 5 is increased, resulting in increased heat and reduce the temperature of the reaction solution.

By reducing the temperature of the reaction solution below 80aboutWith the three way valve 9 reduces the circulating flow of the reaction stream through the heat exchanger 5 and extends through the bypass line 7, which leads to the reduction of heat transfer and temperature rise.

Cyclohexanone in the reactor 1 is supplied through the control valve 16 in the amount of 60-90% of the total facility intake cyclohexasiloxane. This number is calculated by the control system from a condition of maintaining minimum thermal effects on organic products released from the reaction heat.

Circulating the reaction solution is mixed in the reactor 1 with the incoming cyclohexanehexol, in the heat of reactions rearrangements and dissolution of sulfuric anhydride is heated to 90-115aboutC. the Reaction of the that acidity in the reactor 2 is lower than in the reactor 1, to provide the desired viscosity of the circulating reaction solution temperature should be somewhat higher than in the circuit of the reactor 1.

The temperature coming out of the circulation loop reactor 2 reaction solution depends on the load of the installation and the amount fed into the reactor 2 cyclohexasiloxane.

The calculated value of TRasch.temperature entering the reactor 2 flow circulating reaction solution forms a functional unit 22 on the basis of dependencies

TRasch.217,6 258,4 M/(2,2 + G/Gm).

The output signal TRasch.block 22 is slid in function block 23 and to the first input of the regulator 24, the second input of which receives the signal T2from sensor 12 current value of the temperature entering the reactor 2, the reaction solution. The output signal of the controller 24 controls the three-way regulating valve 11, thereby realizing the dependence of T2TRasch.

Despite the fact that T2> T180aboutWith properly selected distribution innings cyclohexasiloxane in reactor 1 and reactor 2 prevents overheating and resinification of organic p. the purpose ground receiving stations unit 20 based on the input humidity setpoints cyclohexasiloxane, r1and r2coefficients of heat generates a signal A (1 )r1+ r2and functional unit 21 on the basis of the input setpoints heat capacity of the reaction solution, G1and G2the volume of circulation in the circuits 1 and 2 reactors respectively generates signals B 1/(cG1and C 1/(cG2and throws in block 25, the signal in the block 26 and the signal B + C

Block 25 multiplication on the basis of the received signals A and B of the blocks 20 and 21, respectively, generates an AC signal, and the block 26 generates a signal A(B + C).

Block 27 multiplication on the basis of the signal G from the flow meter 14 and the AC signal from the output unit 25 generates a signal DAS, which is supplied to the first input of the adder 28.

To the second input of the adder 28 receives the signal D TRasch.80 generated by the functional unit 23 on the basis of the signal TRasch.from the output of block 22.

The output signal GAC + D of the adder 28 is served on the first input (the dividend) block 29 division, to the second input (the divisor) from the output unit 26 receives the signal A(B + C). The output signal (GAC + D)/[A(B + C)] unit 29 division is a signal To control an adjustable valve 16 filing cyclohexasiloxane in the reactor 1, the corresponding optimal supply providing puddleglumfarouk 10000 wt. including cyclohexasiloxane with a moisture content of 4.8 wt. on the installation, including two series-connected reactor with circulating pumps and heat exchangers. The performance of the circulation pumps are the same and equal 386000 wt.h. The molar ratio of sulfuric acid:the oxime support equal of 1.65, which is achieved by applying 13035 wt.h. 20% oleum.

In the first reactor serves 70% of the total cyclohexasiloxane, i.e. 7000 wt.h. The multiplicity of circulation is 386000:(7000 + +13035) 19,3. The temperature of the reaction solution at the inlet to the first reactor support 60aboutWith, and at the entrance to the heat exchanger 83aboutC.

The reaction solution from the first reactor serves the second, which also serves the rest of cyclohexasiloxane, i.e. 3000 wt.h. The multiplicity of the circulation circuit of the second reactor is 386000:(20035 + 3000) 16,8.

Due to the fact that at temperatures below 80aboutWith the speed of the rearrangement reaction is severely reduced, part of the unreacted cyclohexasiloxane comes from the first reactor to the second, thereby increasing the heat removal in the heat exchanger of the second reactor. The temperature at the inlet of the heat exchanger of the second reactor and the outlet thereof is 106 and 90aboutWith according to Avelino significant and is 106 83 23aboutC.

The yield of caprolactam is 96.8% specific consumption of oleum in terms of the monohydrate is to 1.48 t/t caprolactam.

Abruptly reduce the load on the installation cyclohexanehexol to 60% of the original, i.e., serves 6000 Mas.h. cyclohexasiloxane and 7820 wt.h. 20% oleum.

In the first reactor also serves 70% of the total cyclohexasiloxane, i.e. 4200 wt. including a Multiplicity of circulation is 32,1. The temperature of the reaction solution at the inlet to the first reactor 60aboutWith, at the entrance to the heat exchanger of the first reactor 79aboutC. the Ratio of the circulation circuit of the second reactor is 27,9. The temperature of the reaction solution at the inlet to the second reactor 90aboutWith, and at the outlet of the reactor (at the entrance to the heat exchanger) 100aboutC. the difference between the temperature in the reactor is 100 -79 21aboutS, i.e. unbalance thermal reactors is stored and when the load goes from 100% to 60% of nominal.

The yield of caprolactam was 97.4% of the specific consumption of oleum in terms of the monohydrate was 1,43 t/t caprolactam.

P R I m m e R 2. Spend the rearrangement reaction cyclohexasiloxane the same number and composition as in example 1. At the,0. Submission of oleum is carried out in a number of L 0,41100000,9523,2 12490. The molar feed ratio is 1.58.

The temperature of the circulating reaction solution at the inlet to the second reactor support equal

TRasch.217,6 258,41,58/(2,2 + 1,0) 90aboutC.

A (1 )r1+ r2< / BR>
0,952496 + 0,0481128 526,3;

B C 1/(cG1) 1/(0,35386000) 7,410-6;

D TRasch.80 10, and filing cyclohexasiloxane in the first reactor is (GAC + D)/[A(B + C)](10000526,37,410-6+ 10)/(526,327,410-6) 6280.

The multiplicity of circulation is 20.6. The temperature of the reaction solution at the inlet to the first reactor is 80aboutWith, at the exit of the reactor 104,5aboutC.

Rearranged product from the first reactor is fed to the second, which also serves the rest of cyclohexasiloxane, 3720 wt.h. The multiplicity of the circulation circuit of the second reactor is 17.2.

The temperature of the circulating reaction solution at the inlet to the second reactor 90aboutAnd on the exit of 104.5aboutC. the Difference between the values of maximum temperatures in the first and second reactors is less than 0.1aboutC.

The yield of caprolactam amounted to 97.1% specific consumption of oleum in terms of match 60% of the initial maximum load i.e. serves 6000 Mas.h. cyclohexasiloxane and L 0,4160000,9522,8 6560 wt.h. 20% oleum. The molar ratio of the feed at 1.38.

The temperature of the circulating reaction solution at the inlet to the second reactor support equal to the settlement value:

TRasch.217,6 258,41,38/(2,2 + 0,6)90aboutC.

The parameters A,B,C and D remain unchanged, and filing cyclohexasiloxane in the first reactor 4,200 wt.h. The relative amount supplied to the first reactor cyclohexanehexol is accounted for 71.3% of the total number of cyclohexasiloxane received at the installation. The multiplicity of the circulation circuit of the first reactor is 35,6. The temperature of the reaction solution at the inlet to the first reactor is 80aboutAnd on the exit 97aboutC.

Rearranged product from the first reactor is fed to the second, which also serves the rest of cyclohexasiloxane, i.e., 1720 wt.h. The multiplicity of the circulation circuit of the second reactor is 30.7. The temperature of the reaction solution at the inlet to the second reactor 90aboutAnd on the exit 97aboutC. Thus, when the load changes the setup from 100 to 60% balanced temperature reactors is not happening.23 ton/tons of caprolactam.

The results of the examples are summarized in table.

Thus, the average increase in the yield of caprolactam during load fluctuations within 60-100% 0.25% average reduction in consumption of oleum is 0.135 t/t caprolactam.

The application of the method in the manufacture of caprolactam capacity of 60000 tons/year will allow to increase the production of caprolactam 150 t/year and reduce the consumption of oleum by 8,100 tons/year

The PROCESS CONTROL METHOD of OBTAINING CAPROLACTAM by REACTION REARRANGEMENT CYCLOHEXASILOXANE, including the measurement of total consumption cyclohexasiloxane and determination of humidity, measurement of the acidity of the reaction solution and the flow control oleum depending on flow cyclohexasiloxane and acidity of the reaction solution, characterized in that the rearrangement cyclohexasiloxane in caprolactam is carried out in two series-connected reactors with circulating heat exchangers, measure and regulate the temperature of the inputs in the first and second reactors, determine the relative load setup cyclohexanone and the acidity of the solution in the second reactor, adjusting the flow rate of oleum supplied to the first reactor, depending on the relative load actor depending on the total consumption cyclohexasiloxane, served in both reactors, the moisture content in cyclohexanehexol and acidity of the solution in the second reactor, and the temperature of the solution in the second reactor is adjusted depending on the relative load setup cyclohexanehexol and pH in the second reactor.

 

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