CN113477208B - Chloroacetic acid production device and process - Google Patents
Chloroacetic acid production device and process Download PDFInfo
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- CN113477208B CN113477208B CN202110667365.XA CN202110667365A CN113477208B CN 113477208 B CN113477208 B CN 113477208B CN 202110667365 A CN202110667365 A CN 202110667365A CN 113477208 B CN113477208 B CN 113477208B
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Abstract
The invention relates to a chloroacetic acid production device and process, which take acetic acid and chlorine as raw materials, take sulfur as a catalyst, automatically measure acetic acid through a flow meter and feed into an auxiliary reaction kettle, measure sulfur through a measuring tank and feed into the auxiliary reaction kettle, react in the auxiliary reaction kettle and absorb chlorine and generate catalytic reaction, transfer reaction liquid into a main reaction kettle by a pump and introduce chlorine for reaction, blow and purge the reaction liquid to the end point, and then place the reaction liquid into a water distribution tank through a pipeline to prepare an aqueous solution; reaction gas of the main reaction kettle is condensed to recover condensate, and then is connected to an acetic acid washing tower through a pipeline to be washed, and the reaction gas is condensed by a first-stage condenser to recover the condensate and then is subjected to deacidification recovery system to recover acetic acid and hydrochloric acid and ensure that tail gas is discharged after reaching standards. The device and the method match the number of the main kettles and the auxiliary kettles according to the yield requirement, the utilization rate of the continuous feeding and discharging production equipment of the plurality of main kettles and the auxiliary kettles is high, the automation degree is high, the production continuity is high, and the product quality is improved through stable control.
Description
Technical Field
The invention relates to a chloroacetic acid production device, in particular to a novel device for continuously and automatically producing chloroacetic acid by a sulfur catalysis method.
Background
The production of chloroacetic acid by sulfur catalysis method generally adopts an intermittent production process, and the chemical reaction formula is that chloroacetic acid and chlorine gas are prepared in the presence of sulfur to obtain chloroacetic acid and hydrogen chloride gas.
In the production process, two or more reaction kettles are generally adopted, and chlorine is alternately introduced into the reaction kettles for production. The main flow comprises the steps of feeding into a reaction kettle, adding sulfur, absorbing tail gas of a main reaction kettle by an auxiliary reaction kettle, adding acetic acid and sulfur after discharging from the main reaction kettle, switching into the auxiliary reaction kettle, and switching an original auxiliary reaction kettle into the main reaction kettle. The whole production system has poor production continuity and low automation degree, the valves need to be switched repeatedly according to different stages, the production efficiency is low, and the labor intensity is high.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a novel method for producing chloroacetic acid by a sulfur catalysis method, a main reaction kettle and a secondary reaction kettle are fixed, acetic acid and sulfur are directly added into the secondary reaction kettle, a water distribution pipe is placed into the main reaction kettle through a pipeline after the reaction of the main reaction kettle is finished to be added with water to prepare a water solution, materials in the secondary reaction kettle are transferred into the main reaction kettle through a material transfer pump after the discharging for chlorine gas introduction reaction, reaction tail gas is cooled by a primary circulating water heat exchanger and then enters the secondary reaction kettle to absorb excessive chlorine gas, and meanwhile, the tail gas contains chlorine gas and hydrogen chloride as initiators to promote the sulfur to be converted into a catalyst; cooling the tail gas of the secondary reaction kettle by a secondary graphite heat exchanger, and then, washing the tail gas in an acetic acid washing tower to recover the catalyst carried in the tail gas; and cooling the washed tail gas by a brine heat exchanger, allowing the cooled tail gas to enter an acid recovery secondary acetic acid absorption tower for absorbing and recovering acetic acid and a quaternary hydrochloric acid absorption tower for recovering hydrogen chloride to produce a byproduct hydrochloric acid, and allowing the residual tail gas to reach the standard after absorbing the acidic tail gas by an alkali absorption tower and discharging the acidic tail gas.
The invention aims to provide a chloroacetic acid production device, wherein an acetic acid feeding pipe is connected with a top feeding hole of an auxiliary reaction kettle, an upper feeding hole of the auxiliary reaction kettle is connected with a sulfur metering tank, a bottom discharging hole of the auxiliary reaction kettle is connected with an upper inlet of a main reaction kettle through an auxiliary kettle material transferring pump pipeline, a chlorine pipe is connected with an upper air inlet of the main reaction kettle, and a bottom outlet of the main reaction kettle is connected with a feeding hole of a chloroacetic acid water distribution tank through a pipeline.
The main reaction kettle is of a multi-stage parallel structure. The secondary reaction kettle is of a multistage parallel structure. Each 16 sets of 10000L enamel kettles are connected in parallel to form a main kettle, 6 sets of 10000L enamel kettles are connected in parallel to form an auxiliary kettle, and 1 set of acetic acid washing tower and acetic acid washing tank are connected in parallel; each main kettle is provided with 2 graphite heat exchangers of 40 square meters,
the gas outlet of the main reaction kettle is connected with the gas inlet at the upper part of the main kettle one-level tail gas condenser, the gas outlet at the lower part of the main kettle one-level tail gas condenser is connected with the gas inlet of the main kettle two-level tail gas condenser, and the gas outlet of the main kettle two-level tail gas condenser is connected with the auxiliary reaction kettle through a pipeline.
And a tail gas outlet of the auxiliary reaction kettle is connected with an upper air inlet of an auxiliary kettle first-stage tail gas condenser, a lower air outlet of the auxiliary reaction kettle first-stage tail gas condenser is connected with an upper air inlet of an auxiliary reaction kettle second-stage tail gas condenser, and a lower air outlet of the auxiliary reaction kettle second-stage tail gas condenser is connected with a lower air inlet of an acetic acid washing tower.
An air outlet at the upper part of the acetic acid washing tower is connected with the upper part of an acetic acid tail gas washing condenser, the bottom of the acetic acid washing tower tail gas condenser is connected with an acetic acid washing tank through a pipeline, and the lower part of the acetic acid washing tower tail gas condenser is connected to a tail gas recovery device.
A feeding hole in the top of the acetic acid washing tank is connected with an acetic acid feeding pipe, an outlet in the bottom of the acetic acid washing tank is connected with a feeding hole in the top of the acetic acid washing tower through a circulating pump of the washing tower, and a discharging hole in the bottom of the acetic acid washing tank is connected with an inlet in the upper part of the acetic acid washing tank; and simultaneously, a discharge port at the bottom of the acetic acid washing tank is connected with a feed inlet of the main reaction kettle through an auxiliary kettle transfer pump pipeline.
The discharge port at the bottom of the auxiliary reaction kettle is connected with the inlet at the upper part of the auxiliary reaction kettle through a pipeline of an auxiliary kettle material transferring pump.
The lower discharge port of the primary tail gas condenser of the main kettle is connected with the lower discharge port of the secondary tail gas condenser of the main kettle and is connected with the upper feed port of the main reaction kettle through a pipeline.
The lower discharge port of the secondary reaction kettle first-stage tail gas condenser is connected with the lower discharge port of the secondary reaction kettle second-stage tail gas condenser and is connected with the upper feed port of the secondary reaction kettle through a pipeline.
A production process of chloroacetic acid comprises the following steps:
(1) Adding a certain amount of acetic acid into the secondary reaction kettle, and adding sulfur through a sulfur metering tank;
(2) Transferring the materials in the auxiliary reaction kettle into the main reaction kettle through a material transferring pump, and introducing chlorine gas to react to produce chloroacetic acid after the material transferring of the auxiliary reaction kettle is finished and the feeding of the main reaction kettle is finished;
(3) After the reaction of the materials is finished, purging the materials by using nitrogen to remove HCl and chlorine in the reaction liquid; after the purging is finished, the negative pressure is pumped by a water distribution tank, the materials are placed in the water distribution tank and added with water to prepare an aqueous solution, and the aqueous solution is pumped to a chloroacetic acid storage tank; the reaction gas of the main reaction kettle condenses volatile materials in the gas through a primary tail gas condenser of the main reaction kettle and a secondary tail gas condenser of the main reaction kettle, the condensed materials enter the main reaction kettle through a return pipe, and the uncondensed gas enters the auxiliary reaction kettle after being gathered through a pipeline;
(4) The secondary reaction kettle absorbs unreacted chlorine and hydrogen chloride generated by the main reaction kettle, the chlorine chloride and the hydrogen chloride react with sulfur to generate disulfide dichloride, the disulfide dichloride and acetic acid react to generate acetyl chloride (catalyst), the consumption of the chlorine is effectively reduced, the environmental protection risk caused by excessive chlorine and incapability of absorbing is reduced, and the generated catalyst is beneficial to the continuous reaction of the main reaction kettle; after the reaction, the gas is condensed by a first-stage tail gas condenser of the auxiliary kettle and a second-stage tail gas condenser of the auxiliary kettle, the condensed material enters the auxiliary reaction kettle through a return pipe, and the gas which is not condensed enters an acetic acid washing tower through a pipeline;
(5) And (3) the tail gas of the secondary reaction kettle enters an acetic acid washing tower, catalytic substances in the tail gas are washed by acetic acid, the catalyst in the tail gas is recovered, the washed tail gas is condensed by a tail gas condenser of the washing tower, the uncondensed tail gas is conveyed to an acid recovery process through a pipeline, and acetic acid and a byproduct hydrochloric acid are recovered.
The acetic acid in the acetic acid washing tower is circulated acetic acid in the acetic acid washing tank, namely the acetic acid is added into the acetic acid washing tank by controlling a constant liquid level by a liquid level meter of the acetic acid washing tank (12) and is sequentially added into the acetic acid washing tower to absorb tail gas from the secondary reaction kettle; after absorbing the tail gas, the acetic acid washing tower transfers the condensate into an acetic acid washing tank.
The feeding ratio of sulfur to acetic acid in the secondary reaction kettle is 0.017-0.023, the reaction temperature of the secondary reaction kettle is controlled at 45-60 DEG C
After the materials in the auxiliary reaction kettle are added into the main reaction kettle, controlling the temperature in the main reaction kettle to be 60-80 ℃, and controlling the addition amount of chlorine to be 20-100m for ethanol distillation/h; after the reaction is carried out for 5-6 hours, controlling the temperature in the main reaction kettle to be 80-90 ℃ and the chlorine addition amount to be 100-150m for carrying out dry distillation/h; and after the reaction is carried out for 10 hours, controlling the temperature in the main reaction kettle to be 90-105 ℃, and carrying out the dry distillation at the chlorine addition amount of 150-20 m/h.
The acetic acid washing tank is controlled by a liquid level meter to be in a constant liquid level and is pumped into the main reaction kettle. Adding acetic acid into an acetic acid washing tank, controlling the flow rate to be 15-20 m/h through a circulating pump for circulation, and intercepting the acetyl chloride catalyst which is not condensed in the side reaction kettle; simultaneously interior material does not contain the solid material of sulphur and absorbs and dissolves hydrogen chloride, and difficult cooling crystallization can regard as the pipeline flushing medium, and after the auxiliary reaction cauldron feeding, in sending the main reation kettle with fixed amount of material to the pump through flow measurement with single batch, wash auxiliary reaction cauldron and advance the main reation kettle pipeline, prevent that the sulphur deposit from causing the pipe blockage.
The production method can be matched with the number of the main reaction kettle and the auxiliary reaction kettle according to production requirements, and the production is interlocked with the pneumatic regulating valve and the pneumatic switch valve by utilizing liquid level, temperature, flow and the like to automatically switch feeding and discharging, so that the automatic control of the system is improved, and the continuous and stable operation of the system is ensured.
The method has the following advantages:
(1) The automation degree of the equipment is high, automatic control can be realized, and the labor intensity of personnel is effectively reduced.
(2) The device can increase the utilization rate of equipment, and the equipment investment of a batch process designed with the same yield can be reduced by 20 percent.
(3) The method can effectively improve the production stability, ensure the stable auxiliary kettle time, realize the refined control of the temperature and chlorine flux of the whole reaction flow through the detection of an electronic instrument and the control of a field valve of a computer system, effectively improve the monochloroacetic acid content of the product and reduce the consumption of acetic acid.
Drawings
FIG. 1 is a structural diagram of a chloroacetic acid production device, wherein 1, a main reaction kettle, 2, a main kettle first-stage tail gas condenser, 3, a main kettle second-stage tail gas condenser, 4, an auxiliary reaction kettle, 5, a sulfur metering tank, 6, an auxiliary kettle first-stage tail gas condenser, 7, an auxiliary kettle second-stage tail gas condenser, 8, an auxiliary kettle material transfer pump, 9, an acetic acid washing tower, 10, a washing tower circulating pump, 11, a washing tower tail gas condenser and 12, an acetic acid washing tank.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
The utility model provides a chloroacetic acid apparatus for producing, the acetic acid inlet pipe links to each other with 4 top feed inlets of auxiliary reaction cauldron, and 4 upper portion feed inlets of auxiliary reaction cauldron link to each other with sulphur metering tank 5, and 4 bottom discharge mouths of auxiliary reaction cauldron pass through 8 pipe connection main reaction cauldron upper portion imports of auxiliary reaction cauldron material transfer pump, and the chlorine pipe links to each other with 1 upper portion air inlet of main reaction cauldron, and 1 bottom export of main reaction cauldron passes through pipe connection chloroacetic acid water distribution jar feed inlet.
The gas outlet of the main reaction kettle 1 is connected with the gas inlet at the upper part of the main kettle one-level tail gas condenser 2, the gas outlet at the lower part of the main kettle one-level tail gas condenser 2 is connected with the gas inlet of the main kettle two-level tail gas condenser 3, and the gas outlet of the main kettle two-level tail gas condenser 3 is connected with the auxiliary reaction kettle 4 through a pipeline.
4 tail gas outlets of auxiliary reaction cauldron link to each other with 6 upper portion air inlets of auxiliary reaction cauldron one-level tail gas condenser, 6 lower part gas outlets of auxiliary reaction cauldron one-level tail gas condenser link to each other with 7 upper portion air inlets of auxiliary reaction cauldron second grade tail gas condenser, and 7 lower part gas outlets of auxiliary reaction cauldron second grade tail gas condenser link to each other with the air inlet of 9 lower parts of acetic acid scrubbing tower.
An air outlet at the upper part of the acetic acid washing tower 9 is connected with the upper part of an acetic acid tail gas washing condenser 11, the bottom of the acetic acid washing tower tail gas condenser 11 is connected with an acetic acid washing tank 12 through a pipeline, and the lower part of the acetic acid washing tower tail gas condenser 11 is connected with a tail gas recovery device.
A top feeding hole of the acetic acid washing tank 12 is connected with an acetic acid feeding pipe, a bottom outlet of the acetic acid washing tank 12 is connected with a top feeding hole of the acetic acid washing tower 9 through a washing tower circulating pump 10, and a bottom discharging hole of the acetic acid washing tower 9 is connected with an upper inlet of the acetic acid washing tank 12; and simultaneously, a discharge port at the bottom of the acetic acid washing tank 12 is connected with a feed inlet of the main reaction kettle 1 through a pipeline of an auxiliary kettle transfer pump 8.
The discharge port at the bottom of the auxiliary reaction kettle 4 is connected with the inlet at the upper part of the auxiliary reaction kettle 4 through a pipeline of an auxiliary kettle material transferring pump 8.
The lower discharge port of the main kettle first-stage tail gas condenser 2 is connected with the lower discharge port of the main kettle second-stage tail gas condenser 3 and is connected with the upper feed port of the main reaction kettle 1 through a pipeline.
The lower discharge port of the secondary reaction kettle first-stage tail gas condenser 6 is connected with the lower discharge port of the secondary reaction kettle second-stage tail gas condenser 7 and is connected with the upper feed port of the secondary reaction kettle 4 through a pipeline.
Example 2
Taking annual 6 ten thousand tons/year chloroacetic acid production as an example, a production device needs to be provided with 16 sets of 10000L enamel kettles which are connected in parallel to form a main kettle, 6 sets of 10000L enamel kettles which are connected in parallel to form an auxiliary kettle, and 1 set of acetic acid washing tower and acetic acid washing tank; each main kettle is provided with 2 graphite heat exchangers of square meter of 40, the cooling medium of the primary condenser of the main kettle is circulating water, and the secondary condenser of the main kettle adopts frozen salt water of minus 15 ℃ as the cooling medium; the main kettle is provided with a feeding switch valve for controlling the automatic feeding of the main kettle, the main kettle is provided with a discharging switch valve for controlling the automatic discharging of the main kettle after the reaction is finished, the main kettle is provided with an electronic hydrometer, a chlorine flowmeter and a chlorine feeding regulating valve, the reaction process is controlled by monitoring the material specific gravity, and the chlorine flow is automatically regulated; the main reaction kettle is provided with a jacket water inlet regulating valve, a water outlet switch valve, a water inlet steam regulating valve and a water discharge switch valve, and the reaction temperature is automatically regulated according to the reaction process; each set of secondary reaction kettle is provided with 2 graphite heat exchangers with the size of 40 square meters, the cooling medium of a primary condenser is circulating water, and a secondary condenser adopts frozen salt water with the temperature of-15 ℃ as a cooling medium; the auxiliary kettle is provided with a jacket steam inlet regulating valve, and the steam inlet is automatically controlled to regulate the temperature of the auxiliary kettle during reaction; the feeding of the auxiliary kettles is matched with a mass flow meter, each set of auxiliary reaction kettle is matched with a feeding switch valve, and 7.5 tons of acetic acid feeding materials are fixed in a single batch; the secondary reaction kettle is provided with a sulfur metering tank and a sulfur feeding switch valve, and 160kg of sulfur is metered in a single batch; the secondary reaction kettle is provided with a pressure gauge, a tail gas inlet switch valve, a secondary condenser and a tail gas emptying valve and a vacuum regulating valve, the secondary reaction kettle is automatically switched to a vacuum pumping state after the feeding is finished, and a sulfur metering tank valve is opened after the pressure is-0.04 MPa to supplement nitrogen for automatic feeding; after the feeding is finished, the production state of the secondary reaction kettle is switched; carrying out automatic circulation absorption on low-boiling-point substances carried in tail gas by using a circulation pump on an acetic acid washing tank and an acetic acid washing tower, controlling the circulation flow at 20 m/h, carrying out condensation on the tail gas by using a 100 square meter graphite heat exchanger behind the absorption tower and using frozen brine at the temperature of-15 ℃, and recycling a condensate liquid in the acetic acid washing tank; the washing tank is provided with a radar liquid level meter and a feeding switch valve, and the liquid level stability of the washing tank is automatically controlled; controlling the temperature of the auxiliary reaction kettle to be 55 ℃, controlling the chlorine introduction amount to be 20m for carrying out the high-pressure distillation at 50 ℃ when the main reaction kettle starts chlorine introduction, and regulating the chlorine introduction amount to be 30m for carrying out the high-pressure distillation at 55 ℃ after half an hour of chlorine introduction; controlling the chlorine introduction amount to 40m for carrying out the high-speed plantation/h after the chlorine introduction is carried out for 1 hour, and controlling the temperature to be 60 ℃; after chlorine introduction for 2 hours, controlling the chlorine introduction amount to be 60 m/h and controlling the temperature to be 65 ℃; after chlorine is introduced for 3 hours, the temperature is controlled to be 70 ℃; after the chlorine passing amount is 4 hours, controlling the chlorine passing amount to be 80 m/h, and controlling the temperature to be 75 ℃; after the chlorine passing amount is 5 hours, controlling the chlorine passing amount to be 100 m/h, and controlling the temperature to be 80 ℃; after the chlorine passing amount is 6 hours, controlling the chlorine passing amount to be 120 m/h, and controlling the temperature to be 82 ℃; after chlorine introduction for 7 hours, controlling the chlorine introduction amount to be 150 m/h and controlling the temperature to be 85 ℃; carrying out the reaction for 8-13 hours, controlling the chlorine content to be 150 m/h, and controlling the temperature to be 90 ℃; carrying out the reaction for 14-18 hours, controlling the chlorine introduction amount to be 150 m/h, and controlling the temperature to be 95 ℃; after 18 hours of reaction, controlling the chlorine introduction amount to be 120m for carrying out dry harvest/h and controlling the temperature to be 96 ℃; after reacting for 19 hours, controlling the chlorine introduction amount to be 90m for carrying out the high-pressure distillation/h and controlling the temperature to be 98 ℃; after 20 hours of reaction, controlling the chlorine introduction amount to be 70m for carrying out dry harvest/h and controlling the temperature to be 99 ℃; after 21 hours of reaction, controlling the chlorine introduction amount to be 50m for carrying out dry harvest/h and controlling the temperature to be 100 ℃; after 22 hours of reaction, controlling the chlorine introduction amount to be 30m for carrying out dry harvest/h and controlling the temperature to be 102 ℃; reacting for 23 hours, stopping introducing chlorine, and producing about 11.8 tons of chloroacetic acid stock solution products with chloroacetic acid content of 94.0 percent, dichloroacetic acid content of 3.3 percent and acetic acid content of 0.7 percent; the product is prepared into a chloroacetic acid solution product with 75% of monochloroacetic acid, 2.6% of dichloroacetic acid and 0.5% of acetic acid by adding water. After the discharge of the main reaction kettle is finished, the system automatically opens a corresponding auxiliary kettle discharge valve and a corresponding main kettle feed valve needing feeding according to the auxiliary kettle number, and starts a material transferring pump to automatically transfer the materials in the auxiliary kettle into the main kettle; after the material transfer of the auxiliary kettle is finished, a series valve between the bottom of the washing tank and the auxiliary kettle is automatically opened, the flow is controlled to automatically transfer 0.5 ton to the main kettle, and a feeding pipeline is flushed; the auxiliary kettle discharges materials according to numbers to realize first-in first-out and control production according to fixed flow, thus realizing the automatic continuous production of the system.
Example 3
The device can improve the capacity of the device by increasing the number of the main kettles and the auxiliary kettles in the same proportion, taking the annual production of 8 ten thousand tons/year chloroacetic acid (counted by 330 days of annual production), the production device needs to be provided with 22 sets of 10000L enamel kettles which are connected in parallel to form the main kettle, 9 sets of 10000L enamel kettles which are connected in parallel to form the auxiliary kettle, and 1 set of acetic acid washing tower and acetic acid washing tank; each main kettle is provided with 2 square meter graphite heat exchangers of 40, the cooling medium of the primary condenser of the main kettle is circulating water, and the secondary condenser of the main kettle adopts frozen salt water of-15 ℃ as the cooling medium; the main kettle is provided with a feeding switch valve for controlling the automatic feeding of the main kettle, a discharging switch valve for controlling the automatic discharging of the main kettle after the reaction is finished, and an electronic proportion meter, a chlorine flow meter and a chlorine feeding regulating valve for controlling the reaction process and automatically regulating the chlorine flow by monitoring the material proportion; the main reaction kettle is provided with a jacket water inlet regulating valve, a water outlet switch valve, a water inlet steam regulating valve and a water discharge switch valve, and the reaction temperature is automatically regulated according to the reaction process; each set of secondary reaction kettle is provided with 2 graphite heat exchangers with the size of 40 square meters, the cooling medium of a primary condenser is circulating water, and a secondary condenser adopts frozen salt water with the temperature of-15 ℃ as a cooling medium; the auxiliary kettle is provided with a jacket steam inlet regulating valve, and the temperature of the auxiliary kettle is regulated by automatically controlling steam feeding during reaction; the feeding of the auxiliary kettles is matched with a mass flow meter, each set of auxiliary reaction kettle is matched with a feeding switch valve, and 7.6 tons of acetic acid feeding materials are fixed in a single batch; the secondary reaction kettle is provided with a sulfur metering tank and a sulfur feeding switch valve, and 170kg of sulfur is metered in a single batch; the secondary reaction kettle is provided with a pressure gauge, a tail gas inlet switch valve, a secondary condenser and a tail gas emptying valve and a vacuum regulating valve, the secondary reaction kettle is automatically switched to a vacuum pumping state after the feeding is finished, and a sulfur metering tank valve is opened after the pressure is-0.04 MPa to supplement nitrogen for automatic feeding; after the feeding is finished, the production state of the secondary reaction kettle is switched; carrying out automatic circulation absorption on low-boiling-point substances carried in tail gas by using a circulation pump arranged in an acetic acid washing tank and an acetic acid washing tower, controlling the circulation flow at 20 m/h, carrying out condensation on the tail gas by using a 120-square meter graphite heat exchanger arranged behind the absorption tower and using frozen brine at the temperature of-15 ℃, and recycling a condensate liquid in the acetic acid washing tank; the washing tank is provided with a radar liquid level meter and a feeding switch valve, and the liquid level stability of the washing tank is automatically controlled; controlling the automatic control temperature of the auxiliary reaction kettle to be 55 ℃, automatically controlling the chlorine introducing amount and the reaction temperature of the main reaction kettle through a system, controlling the chlorine introducing amount to be 20 m/h and the temperature to be 50 ℃ when the main reaction kettle starts chlorine introducing, and regulating the chlorine introducing amount to be 30 m/h after half an hour of chlorine introducing and temperature to be 55 ℃; controlling the chlorine introduction amount to 40m for carrying out the high-speed plantation/h after the chlorine introduction is carried out for 1 hour, and controlling the temperature to be 60 ℃; after chlorine introduction for 2 hours, controlling the chlorine introduction amount to be 60 m/h and controlling the temperature to be 65 ℃; after chlorine is introduced for 3 hours, the temperature is controlled to be 70 ℃; after the chlorine passing amount is 4 hours, controlling the chlorine passing amount to be 80 m/h, and controlling the temperature to be 75 ℃; after the chlorine passing amount is 5 hours, controlling the chlorine passing amount to be 100 m/h, and controlling the temperature to be 80 ℃; after the chlorine passing amount is 6 hours, controlling the chlorine passing amount to be 120 m/h, and controlling the temperature to be 82 ℃; after chlorine introduction for 7 hours, controlling the chlorine introduction amount to be 150 m/h, and controlling the temperature to be 85 ℃; carrying out the reaction for 8-13 hours, controlling the chlorine content to be 150 m/h, and controlling the temperature to be 90 ℃; carrying out the reaction for 14-18 hours, controlling the chlorine introduction amount to be 150 m/h, and controlling the temperature to be 95 ℃; after 18 hours of reaction, controlling the chlorine introduction amount to be 120m for carrying out dry harvest/h and controlling the temperature to be 96 ℃; after reacting for 19 hours, controlling the chlorine introduction amount to be 90m for carrying out the high-pressure distillation/h and controlling the temperature to be 98 ℃; after the reaction is carried out for 20 hours, the chlorine introduction amount is controlled to be 70 m/h, and the temperature is controlled to be 99 ℃; after 21 hours of reaction, controlling the chlorine introduction amount to be 50m for carrying out dry harvest/h and controlling the temperature to be 100 ℃; after 22 hours of reaction, controlling the chlorine introduction quantity to be 30 m/h, and controlling the temperature to be 102 ℃; reacting for 23 hours, stopping introducing chlorine, and producing about 12 tons of chloroacetic acid stock solution products with chloroacetic acid content of 94.0 percent, dichloroacetic acid content of 3.3 percent and acetic acid content of 0.7 percent; the product is prepared into a chloroacetic acid solution product with 75 percent of monochloroacetic acid, 2.6 percent of dichloroacetic acid and 0.5 percent of acetic acid by adding water. After the discharge of the main reaction kettle is finished, the system automatically opens a corresponding auxiliary kettle discharge valve and a corresponding main kettle feed valve needing feeding according to the auxiliary kettle number, and starts a material transferring pump to automatically transfer the materials in the auxiliary kettle into the main kettle; after the material transfer of the auxiliary kettle is finished, a series valve between the bottom of the washing tank and the auxiliary kettle is automatically opened, the flow is controlled to automatically transfer 0.6 ton to the main kettle, and a feeding pipeline is flushed; the auxiliary kettle discharges materials according to numbers to realize first-in first-out, and the production is controlled according to fixed flow, so that the system realizes automatic continuous production. In this embodiment, 6 main kettles and 3 auxiliary kettles are added compared with example 2, and the single batch charging amount is increased by 0.2 ton, so that the yield of each batch can be increased to 12 tons, and the yield of each production year can be increased by 2.3 ten thousand tons.
Example 4
The method and the steps are the same as those in the embodiment 3, only the automatic temperature control of the auxiliary reaction kettle is controlled to be 50 ℃, the chlorine introducing amount and the reaction temperature of the main reaction kettle are automatically controlled through a system, when the main reaction kettle starts chlorine introducing, the chlorine introducing amount is controlled to be 20 m/h, the temperature is controlled to be 53 ℃, the chlorine introducing amount is adjusted to be 30 m/h after half an hour of chlorine introducing, and the temperature is controlled to be 55 ℃; introducing chlorine for 1 hour, controlling the introduction chlorine quantity to be 40 m/h, and controlling the temperature to be 60 ℃; 2 hours after chlorine introduction, controlling the chlorine introduction quantity to be 60 m/h and controlling the temperature to be 65 ℃; after chlorine is introduced for 3 hours, the temperature is controlled to be 70 ℃; after the chlorine passing amount is 4 hours, controlling the chlorine passing amount to be 80 m/h, and controlling the temperature to be 75 ℃; after the chlorine passing amount is 5 hours, controlling the chlorine passing amount to be 100 m/h, and controlling the temperature to be 80 ℃; after the chlorine passing amount is 6 hours, controlling the chlorine passing amount to be 120 m/h, and controlling the temperature to be 82 ℃; after chlorine introduction for 7 hours, controlling the chlorine introduction amount to be 140 m/h, and controlling the temperature to be 85 ℃; carrying out the reaction for 8-13 hours, controlling the chlorine content to be 140 m/h, and controlling the temperature to be 90 ℃; reacting for 14-19 hours, controlling the chlorine introduction quantity to be 140 m/h, and controlling the temperature to be 93 ℃; after the reaction is carried out for 19 hours, controlling the chlorine introduction amount to be 120m for carrying out the high-pressure distillation/h and controlling the temperature to be 95 ℃; after 20 hours of reaction, controlling the chlorine introduction amount to be 90m for carrying out the high-pressure distillation/h and controlling the temperature to be 98 ℃; after 21 hours of reaction, controlling the chlorine introduction amount to be 70m for carrying out dry harvest/h and controlling the temperature to be 99 ℃; after 22 hours of reaction, controlling the chlorine introduction amount to be 50m for carrying out dry harvest/h and controlling the temperature to be 100 ℃; after the reaction is carried out for 23 hours, the chlorine introduction amount is controlled to be 30 m/h, and the temperature is controlled to be 102 ℃; after 24 hours of reaction, the chlorine introduction is stopped, and about 12.1 tons of chloroacetic acid stock solution products with 94.5 percent of monochloroacetic acid, 3.0 percent of dichloroacetic acid and 0.5 percent of acetic acid are produced. According to the requirement and the air temperature, the product is prepared into a chloroacetic acid solution product with 75% of monochloroacetic acid, 2.4% of dichloroacetic acid and 0.6% of acetic acid by adding water, or a chloroacetic acid solution product with 78% of monochloroacetic acid, 2.7% of dichloroacetic acid and 0.5% of acetic acid. The material loss is reduced by increasing the addition of acetic acid and reducing the temperature of the auxiliary kettle, and the monochloroacetic acid content of the chloroacetic acid product is increased by gradually adjusting the chlorine passing amount and the reaction temperature according to the reaction process; the quality of the product is improved, the yield of a single batch can be increased, and the consumption of raw materials is effectively reduced.
Example 5
The method and the steps are the same as those of example 3, only the temperature of the auxiliary reaction kettle is controlled to be 50 ℃, the chlorine introducing amount and the reaction temperature of the main reaction kettle are automatically controlled by a system, when the main reaction kettle starts chlorine introduction, the chlorine introducing amount is controlled to be 20m during flowering/h, the temperature is controlled to be 53 ℃, the chlorine introducing amount is adjusted to be 40m during flowering/h after half an hour of chlorine introduction, and the temperature is controlled to be 55 ℃; carrying out the chlorine introduction amount of 60m and controlling the temperature to be 60 ℃ after the chlorine introduction for 1 hour; after chlorine introduction for 2 hours, controlling the chlorine introduction amount to be 80 m/h and controlling the temperature to be 65 ℃; 3 hours after chlorine introduction, controlling the chlorine introduction quantity to be 100 m/h and controlling the temperature to be 68 ℃; after the chlorine passing amount is 4 hours, controlling the chlorine passing amount to be 120 m/h, and controlling the temperature to be 72 ℃; after the chlorine passing amount is 5 hours, controlling the chlorine passing amount to be 140 m/h, and controlling the temperature to be 78 ℃; after the chlorine passing amount is 6 hours, controlling the chlorine passing amount to be 150 m/h; carrying out the reaction for 7-11 hours, controlling the chlorine content to be 150 m/h, and controlling the temperature to be 85 ℃; carrying out the reaction for 12-17 hours, controlling the chlorine content to be 150 m/h, and controlling the temperature to be 90 ℃; after 18 hours of reaction, controlling the chlorine introduction amount to be 120m for carrying out dry harvest/h and controlling the temperature to be 94 ℃; after reacting for 19 hours, controlling the chlorine introduction amount to be 90m for carrying out the high-pressure distillation at the temperature of 95 ℃; after the reaction is carried out for 20 hours, the chlorine introduction amount is controlled to be 70 m/h, and the temperature is controlled to be 96 ℃; after 21 hours of reaction, controlling the chlorine introduction amount to be 50m for carrying out the high-yield cultivation at 98 ℃; after 22 hours of reaction, controlling the chlorine introduction amount to be 30m for carrying out dry harvest/h and controlling the temperature to be 100 ℃; after the reaction is carried out for 23.5 hours, stopping introducing chlorine, and producing about 12.2 tons of chloroacetic acid stock solution products with the chloroacetic acid content of 95.0 percent, the dichloroacetic acid content of 2.3 percent and the acetic acid content of 0.7 percent; the product is prepared into a chloroacetic acid solution product with 78% of monochloroacetic acid, 1.8% of dichloroacetic acid and 0.5% of acetic acid by adding water. The temperature of the auxiliary kettle is reduced through control, the chlorine flux of the reaction in the early stage of the reaction is controlled, the reaction temperature and the reaction time are reduced, the content of the chloroacetic acid product, namely the monochloroacetic acid, can be increased, the quality of the product is improved, and the consumption of raw materials is effectively reduced.
Example 6
The method and the steps are the same as those of example 3, only the temperature of the auxiliary reaction kettle is controlled to be 48 ℃, the chlorine introducing amount and the reaction temperature of the main reaction kettle are automatically controlled by a system, when the main reaction kettle starts chlorine introduction, the chlorine introducing amount is controlled to be 20m during flowering/h, the temperature is controlled to be 53 ℃, the chlorine introducing amount is adjusted to be 30m during flowering/h after half an hour of chlorine introduction, and the temperature is controlled to be 55 ℃; introducing chlorine for 1 hour, controlling the introduction chlorine quantity to be 50 m/h, and controlling the temperature to be 58 ℃; after chlorine introduction for 2 hours, controlling the chlorine introduction amount to be 70 m/h and controlling the temperature to be 63 ℃; 3 hours after chlorine introduction, controlling the chlorine introduction amount to be 90 m/h, and controlling the temperature to be 68 ℃; after the chlorine passing amount is 4 hours, controlling the chlorine passing amount to be 110 m/h, and controlling the temperature to be 72 ℃; after the chlorine passing amount is 5 hours, controlling the chlorine passing amount to be 130 m/h, and controlling the temperature to be 78 ℃; after the chlorine passing amount is 6 hours, controlling the chlorine passing amount to be 150 m/h; carrying out the reaction for 7-11 hours, controlling the chlorine content to be 160m and controlling the temperature to be 85 ℃; reacting for 12-16 hours, controlling the chlorine introduction quantity to be 160 m/h, and controlling the temperature to be 90 ℃; after the reaction is carried out for 17 hours, the chlorine introduction amount is controlled to be 120 m/h, and the temperature is controlled to be 95 ℃; after the reaction is carried out for 18 hours, the chlorine introduction amount is controlled to be 90 m/h, and the temperature is controlled to be 96 ℃; after reacting for 19 hours, controlling the chlorine introduction amount to be 70m for carrying out dry harvest/h and controlling the temperature to be 96 ℃; after 20 hours of reaction, controlling the chlorine introduction amount to be 50m for carrying out the high-yield cultivation at 98 ℃; after 20.5 hours of reaction, controlling the chlorine introduction amount to be 30 m/h and controlling the temperature to be 100 ℃; reacting for 21.5 hours, stopping introducing chlorine, and producing about 12.3 tons of chloroacetic acid stock solution products with the chloroacetic acid content of 95.4 percent, the dichloroacetic acid content of 2.0 percent and the acetic acid content of 0.6 percent; the product can be prepared into a chloroacetic acid solution product with 78% of monochloroacetic acid, 1.6% of dichloroacetic acid and 0.4% of acetic acid by adding water. The content of chloroacetic acid product, namely monochloroacetic acid, can be improved by controlling and increasing the chlorine flux in the middle reaction stage, reducing the temperature of the secondary reaction kettle and the reaction temperature of the main reaction kettle, reducing the reaction time, reducing the loss of the catalyst and the raw materials and simultaneously reducing the loss of the catalyst and the raw materials.
Example 7
The method and the steps are the same as those of the example 3, only the temperature of the auxiliary reaction kettle is controlled to be 50 ℃, the chlorine introducing amount and the reaction temperature of the main reaction kettle are automatically controlled by a system, when the chlorine introducing amount of the main reaction kettle is started, the chlorine introducing amount is controlled to be 50m during carrying out dry top planting/h, and the temperature is controlled to be 60 ℃; controlling the chlorine introduction amount to be 100m for carrying out the high-speed rice plantation/h after the chlorine introduction is carried out for 1 hour, and controlling the temperature to be 80 ℃; carrying out the reaction for 3-10 hours, controlling the chlorine content to be 120 m/h and controlling the temperature to be 85 ℃; carrying out the reaction for 11-15 hours, controlling the chlorine introduction amount to be 150 m/h, and controlling the temperature to be 90 ℃; after the reaction is carried out for 16 hours, controlling the chlorine introduction amount to be 120 m/h and controlling the temperature to be 100 ℃; and controlling the chlorine introduction quantity to be 80 m/h and the temperature to be 102 ℃ when the reaction lasts for 16-19 hours, and producing about 8.5 tons of chloroacetic acid stock solution products with the chloroacetic acid content of 83.2 percent, the dichloroacetic acid content of 8.5 percent and the acetic acid content of 6.3 percent. The chlorine is introduced too fast in the early stage and the later stage, so that the total reaction time can be reduced, but the main content of monochloroacetic acid in the product can be reduced, and meanwhile, the impurity content in the product is high, so that the yield of the product in a single batch is reduced.
Example 8
The method and the steps are the same as the example 3, only the temperature of the auxiliary reaction kettle is controlled to be 50 ℃, the chlorine introducing amount and the reaction temperature of the main reaction kettle are automatically controlled by a system, when the main reaction kettle is started to introduce chlorine, the chlorine introducing amount is controlled to be 50 m/h, the temperature is controlled to be 100 ℃, the reaction is carried out for 22.5 hours, the content of dichloroacetic acid in the produced monochloroacetic acid is more than 10 percent, the content of monochloroacetic acid is less than 80 percent, the product property is unstable, and the qualified product is difficult to obtain.
Claims (10)
1. A chloroacetic acid production process is characterized by comprising the following steps:
(1) Adding a certain amount of acetic acid into the secondary reaction kettle (4), and adding sulfur in a sulfur metering tank (5);
(2) Transferring the materials in the auxiliary reaction kettle (4) into the main reaction kettle (1) through a material transferring pump, and introducing chlorine gas to react to produce chloroacetic acid after the material transferring of the auxiliary reaction kettle is finished and the material feeding of the main reaction kettle (1) is finished;
(3) After the reaction of the materials is finished, purging the materials by using nitrogen to remove HCl and chlorine in the reaction liquid; after the purging is finished, the negative pressure is pumped by a water distribution tank, the materials are placed in the water distribution tank and added with water to prepare an aqueous solution, and the aqueous solution is pumped to a chloroacetic acid storage tank; the reaction gas in the main reaction kettle (1) is condensed by a main kettle first-stage tail gas condenser (2) and a main kettle second-stage tail gas condenser (3), the condensed material enters the main reaction kettle (1) through a return pipe, and the uncondensed gas is gathered through a pipeline and then enters an auxiliary reaction kettle (4);
(4) The secondary reaction kettle (4) absorbs unreacted chlorine gas in the main reaction kettle (1) and hydrogen chloride generated by the main reaction kettle, the chlorine gas and the hydrogen chloride react with sulfur to generate disulfide dichloride, and the disulfide dichloride and acetic acid react to generate acetyl chloride catalyst; after the reaction, the gas is condensed by a first-stage tail gas condenser (6) of the auxiliary kettle and a second-stage tail gas condenser (7) of the auxiliary kettle, the condensed material enters the auxiliary reaction kettle (4) through a return pipe, and the gas which is not condensed enters an acetic acid washing tower (9) through a pipeline;
(5) And (3) enabling tail gas of the secondary reaction kettle (4) to enter an acetic acid washing tower (9) to wash catalytic substances in the tail gas by using acetic acid, recovering a catalyst in the tail gas, condensing the washed tail gas by a tail gas condenser (11) of the washing tower, conveying the uncondensed tail gas to an acid recovery process through a pipeline, and recovering the acetic acid and producing a byproduct hydrochloric acid.
2. The chloroacetic acid production process of claim 1, wherein the acetic acid in the acetic acid washing column (9) is acetic acid recycled in the acetic acid washing tank (12), i.e. acetic acid is added into the acetic acid washing tank (12) and sequentially recycled into the acetic acid washing column (9) for absorbing the tail gas from the secondary reaction kettle (4); after absorbing the tail gas, the acetic acid washing tower (9) transfers the condensate into an acetic acid washing tank (12).
3. The chloroacetic acid production process of claim 1, characterized in that the feeding ratio of sulfur to acetic acid in the secondary reaction kettle (4) is 0.017 to 0.023, and the reaction temperature of the secondary reaction kettle is controlled at 45-60 ℃.
4. The chloroacetic acid production process of claim 1, wherein; after the materials in the secondary reaction kettle (4) are added into the main reaction kettle (1), controlling the temperature in the main reaction kettle (1) to be 60-80 ℃, and controlling the chlorine addition amount to be 20-100m for cultivating each hour; after the reaction is carried out for 5-6 hours, controlling the temperature in the main reaction kettle (1) to be 80-90 ℃ and the chlorine addition amount to be 100-150m for carrying out the downward cultivation/h; after 10 hours of reaction, controlling the temperature in the main reaction kettle (1) to be 90-105 ℃, and carrying out dry distillation at the chlorine addition rate of 150-20 m/h.
5. The chloroacetic acid production process of claim 1, wherein the acetic acid washing tank (12) is operated by acetic acid pump at 15-20 m/h cycle to intercept the acetyl chloride catalyst not condensed in the side reaction kettle.
6. The chloroacetic acid production process of claim 1, wherein the chloroacetic acid production apparatus used for the chloroacetic acid production process comprises an acetic acid feeding pipe connected to a top feeding port of the secondary reaction kettle (4), an upper feeding port of the secondary reaction kettle (4) connected to the sulfur metering tank (5), a bottom discharging port of the secondary reaction kettle (4) connected to an upper inlet of the main reaction kettle (1) through a secondary kettle transfer pump (8) via a pipeline, a chlorine pipe connected to an upper inlet of the main reaction kettle (1), a bottom outlet of the main reaction kettle (1) connected to a feeding port of the chloroacetic acid distribution tank via a pipeline, a tail gas outlet of the secondary reaction kettle (4) connected to an upper inlet of the secondary kettle first-stage tail gas condenser (6), a lower outlet of the secondary kettle first-stage tail gas condenser (6) connected to an upper inlet of the secondary kettle tail gas condenser (7), a lower outlet of the secondary kettle tail gas condenser (7) connected to a lower inlet of the acetic acid washing tower (9), an upper outlet of the acetic acid washing tower (9) connected to an upper outlet of the acetic acid tail gas washing condenser (11), an acetic acid washing tower (11) connected to a top feeding pipe via a gas condenser, an acetic acid washing tower (11) connected to a top washing tank (10), and a top washing tower (10) connected to an acetic acid tail gas recycling pump, a discharge hole at the bottom of the acetic acid washing tower (9) is connected with an inlet at the upper part of the acetic acid washing tank (12); and simultaneously, a discharge port at the bottom of the acetic acid washing tank (12) is connected with a feed port of the main reaction kettle (1) through a pipeline of the auxiliary kettle transfer pump (8).
7. The chloroacetic acid production process of claim 6, wherein an air outlet of the main reaction kettle (1) is connected with an air inlet at the upper part of the main kettle first-stage tail gas condenser (2), an air outlet at the lower part of the main kettle first-stage tail gas condenser (2) is connected with an air inlet of the main kettle second-stage tail gas condenser (3), and an air outlet of the main kettle second-stage tail gas condenser (3) is connected with the auxiliary reaction kettle (4) through a pipeline.
8. The chloroacetic acid production process of claim 7, characterized in that the bottom discharge port of the secondary reaction kettle (4) is connected to the upper inlet of the secondary reaction kettle (4) through the pipeline of the secondary kettle transfer pump (8).
9. The chloroacetic acid production process of claim 7, characterized in that the discharge port at the lower part of the main kettle first stage tail gas condenser (2) is connected with the discharge port at the lower part of the main kettle second stage tail gas condenser (3) and is connected with the feed port at the upper part of the main reaction kettle (1) through a pipeline.
10. The chloroacetic acid production process of claim 6, characterized in that the discharge port at the lower part of the secondary kettle first stage tail gas condenser (6) is connected with the discharge port at the lower part of the secondary kettle second stage tail gas condenser (7) and is connected with the feed port at the upper part of the secondary reaction kettle (4) through a pipeline.
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