CN218609283U - Octyl thioester chloromethyl acid production system - Google Patents

Abstract

The utility model discloses a clomethyl acid octyl thioester production system, including photochemical kettle, be equipped with on the photochemical kettle and add pipeline, catalyst triethylamine and add pipeline, phosgene and add pipeline, nitrogen gas and add pipeline and technology tail gas pipeline to octyl mercaptan, the photochemical kettle is provided with the intermediate layer outward, and interbedded bottom is provided with coolant inlet pipeline, and the top is provided with coolant outlet pipeline, its characterized in that: a flow meter and a flow regulating valve are arranged on the phosgene adding pipeline, the lower end of the phosgene adding pipeline extends to the lower part in the photochemical kettle, the flow meter and the flow regulating valve are arranged on the cooling medium inlet pipeline, a temperature sensor is arranged in the photochemical kettle, automatic control valves are arranged on the nitrogen adding pipeline and the process tail gas pipeline, and the octyl mercaptan adding pipeline and the catalyst triethylamine adding pipeline are respectively connected with the octyl mercaptan metering tank and the triethylamine metering tank. Hot water does not need to be introduced for temperature rise, the dilution of a cooling medium caused by the introduction of the hot water is avoided, and meanwhile, the loss of phosgene is reduced.

Description

Octyl thioester chloromethyl acid production system

Technical Field

The utility model relates to a chemical production technical field, concretely relates to clomethyl acid octyl thioester's synthesis system.

Background

Synthesizing octyl chloromethyl thioester by adopting a phosgene method, adding a certain amount of raw materials Xin Liuzhi and a catalyst (triethylamine) into a photochemical kettle, starting stirring, filling salt water into a jacket for cooling, introducing gaseous phosgene into the photochemical kettle, and reacting octyl mercaptan and phosgene under the action of the catalyst to generate a coarse octyl chloromethyl thioester until phosgene is dropwise added.

In the process of adding phosgene, because the reaction is an exothermic reaction, the current operation is that a cooling medium (calcium chloride aqueous solution, brine is cooled by a uniform refrigeration system and then branched to various uses) is adopted to cool a photochemical kettle, after phosgene is introduced, hot water is introduced into the photochemical kettle and is kept at 40-50 ℃ for reaction till the reaction is complete, photochemical liquid is directly filtered by a filter, and triethylamine hydrochloride generated by filtering is treated as solid waste. Therefore, the problem that the saline water is diluted due to the introduction of hot water, the temperature reduction effect is poor, and the whole refrigeration system is affected exists.

Therefore, a heat preservation kettle is added, after the phosgene is dripped, the reaction liquid is pressed into the heat preservation kettle, hot water is introduced into the heat preservation kettle for heat preservation to 40-50 ℃ for reaction in the heat preservation Wen Fu, and therefore the phenomenon that the saline water is diluted to affect the freezing effect can be avoided.

However, because the boiling point of phosgene is low, the reaction is incomplete when the initial freezing reaction is carried out, the temperature is raised to 40-50 ℃ relatively quickly, phosgene can be partially vaporized and carried away, and the nitrogen pressure is generally adopted when the reaction liquid is fed into a heat preservation kettle, so that the nitrogen can also carry away part of phosgene, and the loss of phosgene is large, therefore, generally, more phosgene is fed, and the amount of phosgene and the weight of octanethiol reach 1:1. Resulting in a large loss of phosgene. With associated greater security risks

SUMMERY OF THE UTILITY MODEL

To the not enough that exists among the prior art, the utility model aims to provide another kind of octyl thioester of chloroformic acid production system does not need the heat preservation cauldron to can reduce the quantity of phosgene.

In order to achieve the above purpose, the utility model adopts the following technical scheme: the production system of octyl thioester of chloroformic acid comprises a photochemical kettle, wherein the photochemical kettle is provided with an octyl mercaptan adding pipeline, a catalyst triethylamine adding pipeline, a phosgene adding pipeline, a nitrogen adding pipeline and a process tail gas pipeline, an interlayer is arranged outside the photochemical kettle, the bottom of the interlayer is provided with a cooling medium inlet pipeline, and the middle upper part of the interlayer is provided with a cooling medium outlet pipeline, and the production system is characterized in that: the system comprises a photochemical kettle, a catalyst triethylamine adding pipeline, a cooling medium inlet pipeline, a temperature sensor, a nitrogen adding pipeline, a catalyst triethylamine adding pipeline and a octyl mercaptan metering tank, wherein the phosgene adding pipeline is provided with a flowmeter and a flow regulating valve, the lower end of the phosgene adding pipeline extends to the lower part in the photochemical kettle, the cooling medium inlet pipeline is provided with a flowmeter and a flow regulating valve, the photochemical kettle is internally provided with a temperature sensor, the nitrogen adding pipeline and the process tail gas pipeline are provided with automatic control valves, and the octyl mercaptan adding pipeline and the catalyst triethylamine adding pipeline are respectively connected with the octyl mercaptan metering tank and the triethylamine metering tank.

By adopting the technical scheme, the flow regulating valve is additionally arranged on the phosgene adding pipeline, the flow of the phosgene can be controlled, and the flow meter can meter the introducing amount of the phosgene.

A flow meter and a flow regulating valve are additionally arranged on an inlet pipeline of the cooling medium, so that the entering amount of the cooling medium can be measured, and the flow of the cooling medium entering the interlayer is regulated through the flow regulating valve.

During reaction, firstly, a flow regulating valve of a cooling medium is fully opened, phosgene is introduced, a large amount of exothermic energy of the reaction is guaranteed to be taken away by saline, the temperature is controlled, when phosgene is introduced to a certain amount, the flow of the cooling medium is adjusted to be small through the flow regulating valve, then when phosgene is introduced to be close to the end sound, the introduction of the cooling medium is stopped, the temperature of a photochemical kettle can be increased to 40-50 ℃ by utilizing reaction heat release, and meanwhile, the introduction amount of the phosgene is adjusted to be small through the flow regulating valve on a phosgene adding pipeline, so that the purpose of controlling the temperature is achieved, and the raw materials are reacted completely. Through process adjustment, the using amount of phosgene is reduced by about 10 percent, the dilution of a cooling medium caused by the fact that hot water is introduced for heating can be avoided, a heat-preservation kettle is reduced, the loss of phosgene is reduced, the product quality is qualified, and the yield is the same as that of the heat-preservation kettle.

After the reaction, introducing nitrogen, taking away unreacted phosgene and hydrogen chloride, introducing the nitrogen to a tail gas destruction tower, adding a phosgene hydrolysis catalyst in the tail gas destruction tower, destroying phosgene, absorbing hydrochloric acid by a water absorption tower and an alkali absorption tower, and discharging, wherein the tail gas treatment is the prior art.

In the scheme, the method comprises the following steps: and the octyl mercaptan adding pipeline and the catalyst triethylamine adding pipeline are provided with automatic control valves, and the octyl mercaptan metering tank and the triethylamine metering tank are respectively connected with the octyl mercaptan storage tank and the triethylamine storage tank through a material transferring pump.

In the scheme, the method comprises the following steps: the photochemical kettle is provided with a liquid outlet pipe used for transferring liquid in the photochemical kettle out to the filter, one end of the liquid outlet pipe, which is positioned in the photochemical kettle, is provided with a filtering sleeve, a plurality of filtering holes are distributed on the filtering sleeve, and a filtering screen is sleeved outside the filtering sleeve. After the reaction is finished, introducing nitrogen into the photochemical kettle to drive phosgene away, introducing the phosgene and the nitrogen into a tail gas destruction tower, and then carrying out water washing, alkali washing and water washing and then discharging.

The liquid outlet pipe is inserted, so that the precipitated triethylamine hydrochloride is directly left in the photochemical kettle without a filter, and the filter is only used for filtering a small amount of residues penetrating through the filter screen. The triethylamine hydrochloride left in the photochemical kettle is directly used as a catalyst. Little or little triethylamine was added later except for the first addition.

Has the advantages that: the utility model discloses an improvement of technology lets in the flow control valve of flow control valve and cooling medium on the pipeline through phosgene, adjusts phosgene and cooling medium's flow, reaches the purpose of controlling temperature in the photochemical kettle. Hot water does not need to be introduced for temperature rise, the dilution of a cooling medium caused by the introduction of the hot water is avoided, and meanwhile, the loss of phosgene is reduced.

Drawings

Fig. 1 is a process flow diagram of the present invention.

Fig. 2 is a schematic view of a structure of the liquid outlet pipe.

Detailed Description

The present invention will be described in further detail with reference to the following embodiments:

example 1

As shown in fig. 1 and 2, a production system of octyl thioester of chloromethyl acid comprises a photochemical kettle 1, wherein the photochemical kettle 1 is provided with a octyl mercaptan adding pipeline, a catalyst triethylamine adding pipeline, a phosgene adding pipeline 101, a nitrogen adding pipeline 102 and a process tail gas pipeline 103, an interlayer is arranged outside the photochemical kettle 1, the bottom of the interlayer is provided with a cooling medium inlet pipeline, the top of the interlayer is provided with a cooling medium outlet pipeline, the photochemical kettle is internally provided with a stirring device, the phosgene adding pipeline is provided with a flow meter 2 and a flow regulating valve 3, the lower end of the phosgene adding pipeline extends to the lower part inside the photochemical kettle 1, the cooling medium pipeline is provided with a flow meter 2 and a flow regulating valve 3, the photochemical kettle 1 is internally provided with a temperature sensor 4, the nitrogen adding pipeline 101 and the process tail gas pipeline 102 are provided with automatic control valves 5, and the octyl mercaptan adding pipeline and the catalyst triethylamine adding pipeline are respectively connected with an octyl mercaptan metering tank 6 and a triethylamine metering tank 7. An automatic control valve 5 is also arranged on the octyl mercaptan adding pipeline and the catalyst triethylamine adding pipeline. And the octyl mercaptan metering tank 6 and the triethylamine metering tank 7 are respectively connected with an octyl mercaptan storage tank 8 and a triethylamine storage tank 9 through a material transfer pump. The octyl mercaptan and the triethylamine in the octyl mercaptan storage tank 8 and the triethylamine storage tank 9 are respectively pumped into respective corresponding metering tanks, and then metered into the photochemical kettle, so that automatic production is realized.

The photochemical kettle 1 is provided with a liquid outlet pipe 10 for transferring liquid in the photochemical kettle to a filter, one end of the liquid outlet pipe 10 positioned in the photochemical kettle 1 is provided with a filtering sleeve 11, a plurality of filtering holes are distributed on the filtering sleeve 11, and a filtering net 12 is sleeved outside the filtering sleeve 11. This part of the disclosure is disclosed in the patent of the applicant's earlier application.

Finally, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the present invention can be modified or replaced by other means without departing from the spirit and scope of the present invention, which should be construed as limited only by the appended claims.

Claims (3)

1. The production system of octyl thioester of chloroformic acid comprises a photochemical kettle, wherein the photochemical kettle is provided with an octyl mercaptan adding pipeline, a catalyst triethylamine adding pipeline, a phosgene adding pipeline, a nitrogen adding pipeline and a process tail gas pipeline, an interlayer is arranged outside the photochemical kettle, the bottom of the interlayer is provided with a cooling medium inlet pipeline, and the middle upper part of the interlayer is provided with a cooling medium outlet pipeline, and the production system is characterized in that: the system comprises a photochemical kettle, a catalyst triethylamine feeding pipeline, a cooling medium inlet pipeline, a nitrogen feeding pipeline, a catalyst triethylamine feeding pipeline, a cooling medium inlet pipeline, a cooling medium outlet pipeline, a catalyst triethylamine feeding pipeline and a temperature sensor, wherein a flowmeter and a flow regulating valve are arranged on the phosgene feeding pipeline, the lower end of the phosgene feeding pipeline extends to the lower part in the photochemical kettle, the flow meter and the flow regulating valve are arranged on the cooling medium inlet pipeline, the temperature sensor is arranged in the photochemical kettle, automatic control valves are arranged on the nitrogen feeding pipeline and the process tail gas pipeline, and the octane mercaptan feeding pipeline and the catalyst triethylamine feeding pipeline are respectively connected with an octane mercaptan metering tank and the triethylamine metering tank.

2. The octyl chlorocarbonate thioester production system according to claim 1, wherein: and the octyl mercaptan adding pipeline and the catalyst triethylamine adding pipeline are provided with automatic control valves, and the octyl mercaptan metering tank and the triethylamine metering tank are respectively connected with the octyl mercaptan storage tank and the triethylamine storage tank through a material transferring pump.

3. The octyl chloroformiate thioester production system according to claim 1 or 2, characterized in that: the photochemical kettle is provided with a liquid outlet pipe used for transferring liquid in the photochemical kettle out to the filter, one end of the liquid outlet pipe, which is positioned in the photochemical kettle, is provided with a filtering sleeve, a plurality of filtering holes are distributed on the filtering sleeve, and a filtering screen is sleeved outside the filtering sleeve.

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