KR102283486B1 - System for munufacturing high purity dimethylamine - Google Patents

Abstract

The present invention relates to a system for manufacturing high purity dimethylamine, and more particularly, to a system for manufacturing high purity dimethylamine, which can improve economic feasibility while obtaining high-purity dimethylamine by using a low-purity dimethylamine product as a raw material and removing impurities contained in the raw material through a low-cost/high-efficiency process. The system according to the present invention comprises: a vaporization unit; an adsorption unit; a specific gravity use processing unit; a cooling unit; and a water removal unit.

Description

High purity dimethylamine manufacturing system {System for munufacturing high purity dimethylamine}

The present invention relates to a high-purity dimethylamine manufacturing system, and more specifically, by using a low-purity dimethylamine product as a raw material and removing impurities contained in the raw material through a low-cost/high-efficiency process, while obtaining high-purity dimethylamine It relates to a high-purity dimethylamine manufacturing system that can improve economic efficiency.

Dimethylamine (DMA) is a colorless gas that smells of fish and shellfish at low concentrations and ammonia at high concentrations. It is widely used when depositing films on wafers during semiconductor processing.

The dimethylamine is generally produced by the catalytic reaction of methanol and ammonia at high temperature and high pressure, as described in the following patent documents.

<Patent Literature>

Patent No. 10-0043886 (registered on August 28, 1991) "Method for producing dimethyl amine"

However, due to the characteristics of the conventional manufacturing process of dimethylamine, it contains a certain amount of impurities such as ammonia and moisture along with the manufactured dimethylamine. There is an impossible problem.

Republic of Korea Patent Publication No. 10-2007-0022779 (2007.02.27.)

The present invention has been devised to solve the above problems,

The present invention uses a low-purity dimethylamine product as a raw material and removes impurities contained in the raw material through a low-cost/high-efficiency process, thereby obtaining high-purity dimethylamine while providing a high-purity dimethylamine manufacturing system with improved economic feasibility. There is this.

In addition, the present invention vaporizes dimethylamine by applying heat to a raw material containing impurities and liquid dimethylamine, removes the remaining liquid dimethylamine, and then adsorbs it, so a high-purity dimethylamine manufacturing system capable of improving the efficiency of adsorption treatment Its purpose is to provide

In addition, the present invention applies heat to liquid dimethylamine temporarily stored in the storage tank to increase the pressure, and the dimethylamine discharged to the storage tank is cooled in the process of passing through the transfer storage unit to reduce the pressure, so that the gas-liquid separation unit without using a pump An object of the present invention is to provide a high-purity dimethylamine manufacturing system that can store dimethylamine from which light impurities have been removed in a storage container.

The present invention is implemented by an embodiment having the following configuration in order to achieve the above object.

According to an embodiment of the present invention, a high-purity dimethylamine manufacturing system according to the present invention includes: a vaporizer for vaporizing dimethylamine by applying heat to a raw material containing impurities and liquid dimethylamine; an adsorption unit for removing impurities by adsorbing the waste product of the vaporization unit containing impurities and gaseous dimethylamine; a specific gravity utilization processing unit for removing impurities from the discharge of the adsorption unit by using the specific gravity difference; a cooling unit for cooling the discharge of the specific gravity utilization processing unit to liquefy dimethylamine in the gaseous phase; and a water removal unit that cools the exhaust from the cooling unit to solidify water to remove water, and wherein the impurities include ammonia, water, monomethylamine, nitrogen and oxygen.

According to another embodiment of the present invention, the high-purity dimethylamine manufacturing system according to the present invention separates the discharge of the water removal unit into vapor phase impurities and liquid dimethylamine, removes vapor phase impurities, and then heats liquid dimethylamine. a gas-liquid separation unit for applying and discharging; and a transfer storage unit for cooling the dimethylamine discharged from the gas-liquid separation unit so that the dimethylamine discharged from the gas-liquid separation unit by the differential pressure can be stored in the storage container.

According to another embodiment of the present invention, in the high-purity dimethylamine manufacturing system according to the present invention, the vaporization part includes a housing forming an outer shape, a raw material transfer tube located inside the housing and moving raw materials, and an end of the raw material transfer tube As the heating medium supplied from the heating medium supply device is supplied into the housing and flows around the raw material transfer tube, including a separator connected to the The liquid dimethylamine is vaporized by heating the raw material transfer tube to transfer heat to the raw material flowing inside, and the raw material discharged from the end of the raw material transfer tube and flowing into the separation unit is separated from the gas and liquid, and the liquid dimethylamine is located on the lower side. , the controller is characterized in that the raw materials except for the liquid dimethylamine are discharged through the upper discharge pipe, and the liquid dimethylamine located at the lower side is sent to the neutralization facility through the lower discharge pipe.

According to another embodiment of the present invention, in the high-purity dimethylamine manufacturing system according to the present invention, the controller checks the level value of dimethylamine in the liquid phase output from the water level sensor located inside the separation unit, and the predetermined level value is abnormal. If it is determined that the raw material is not supplied to the vaporization unit, it is characterized in that the liquid dimethylamine is prevented from being supplied to the adsorption unit.

According to another embodiment of the present invention, in the high-purity dimethylamine manufacturing system according to the present invention, an adsorbent is supported on the adsorbent, and the adsorbent is any one selected from the group consisting of morecuresib, activated carbon and potassium hydroxide. The above is used, and while the discharge of the vaporization unit passes through the adsorption unit, ammonia is mainly removed, and some moisture is removed.

According to another embodiment of the present invention, in the high-purity dimethylamine manufacturing system according to the present invention, the specific gravity utilization processing unit includes a long tower-shaped tower unit, and when the discharge discharged from the adsorption unit flows into the tower unit, The heavy material is located on the lower side and the light material is located on the upper side so that the discharge of the adsorption unit is separated, and the light nitrogen and oxygen are removed while the discharge of the adsorption unit passes through the specific gravity utilization treatment unit.

According to another embodiment of the present invention, in the high-purity dimethylamine manufacturing system according to the present invention, the gas-liquid separation unit includes a storage tank for temporarily storing the discharge of the water removal unit, and a cooling medium or heating medium surrounding the storage tank. A jacket, a vacuum pump connected to the upper side of the storage tank, a discharge pipe connected to the lower end of the storage tank for discharging dimethylamine, and a water level sensor located inside the storage tank to measure the water level therein; The controller operates the cooling medium supply device so that the cooling medium flows through the jacket so that the flow path is smoothed, and the discharge of the water removal unit is supplied to the storage tank, and the controller receives the water level value output from the water level sensor. When it is checked and it is determined that the predetermined water level is abnormal, the discharge is stopped and the discharge is maintained for a predetermined time so that the discharge stored in the storage tank is stabilized so that it is separated into a light upper side impurity and a lower side liquid dimethylamine, and the controller is The vacuum pump is operated to remove the light impurities on the upper side, and the heating medium supply device is operated to allow the heating medium to flow through the jacket. It is characterized in that dimethylamine is discharged through.

According to another embodiment of the present invention, in the high-purity dimethylamine manufacturing system according to the present invention, the dimethylamine discharged from the gas-liquid separation unit has a high pressure, but the dimethylamine that has passed through the transfer storage unit loses heat and has a low pressure , it is characterized in that the liquid dimethylamine that has passed through the transfer storage unit can be stored in the storage container without using a pump due to the pressure difference.

The present invention can obtain the following effects by the present embodiment above.

The present invention uses a low-purity dimethylamine product as a raw material and removes impurities contained in the raw material through a low-cost/high-efficiency process, thereby obtaining high-purity dimethylamine and improving economic efficiency.

In addition, since the present invention vaporizes dimethylamine by applying heat to a raw material containing impurities and liquid dimethylamine and removes the remaining liquid dimethylamine, then adsorption treatment is performed, thereby improving the adsorption treatment efficiency.

In addition, the present invention applies heat to liquid dimethylamine temporarily stored in the storage tank to increase the pressure, and the dimethylamine discharged to the storage tank is cooled in the process of passing through the transfer storage unit to reduce the pressure, so that the gas-liquid separation unit without using a pump There is an effect that dimethylamine from which light impurities have been removed can be stored in a storage container.

1 is a block diagram of a high-purity dimethylamine manufacturing system according to an embodiment of the present invention.
Figure 2 is a detailed configuration diagram for explaining the vaporizer of Figure 1;
3 is a detailed configuration diagram for explaining the adsorption unit, the specific gravity utilization processing unit and the reboiler of FIG. 1 .
4 is a detailed configuration diagram for explaining the cooling unit and the water removal unit of FIG. 1 .
5 is a detailed configuration diagram for explaining the gas phase separation unit of FIG. 1 .
6 is a detailed configuration diagram for explaining the transfer storage unit of FIG.
7 is a flowchart showing a method for preparing high purity dimethylamine according to another embodiment of the present invention.

Hereinafter, a high-purity dimethylamine manufacturing system according to the present invention will be described with reference to the accompanying drawings. Unless otherwise defined, all terms in this specification have the same general meaning as understood by those skilled in the art to which the present invention belongs, and in case of conflict with the meaning of the terms used in this specification, the According to the definition used in the specification. In addition, detailed descriptions of well-known functions and configurations that may unnecessarily obscure the gist of the present invention will be omitted. Throughout the specification, when a part "includes" a certain component, it means that other components may be further included, rather than excluding other components, unless otherwise stated.

1 to 6 of the high-purity dimethylamine manufacturing system according to an embodiment of the present invention, the high-purity dimethylamine manufacturing system vaporizes dimethylamine by applying heat to a raw material containing impurities and liquid dimethylamine. a vaporization unit (1); an adsorption unit (2) for removing impurities by adsorbing the waste product of the vaporization unit containing impurities and gaseous dimethylamine; a specific gravity utilization processing unit 3 for removing impurities from the discharge of the adsorption unit 2 by using the specific gravity difference; a cooling unit (4) for cooling the discharge of the specific gravity utilization processing unit (3) to liquefy dimethylamine in the gaseous phase; a water removal unit (5) for cooling the discharge of the cooling unit (4) to solidify water to remove water; a gas-liquid separation unit 6 that separates the discharge of the water removal unit 5 into vapor phase impurities and liquid dimethylamine, removes vapor phase impurities, and then heats and discharges liquid dimethylamine; a transfer storage unit 7 for cooling the dimethylamine discharged from the gas-liquid separation unit 6 so that the dimethylamine discharged from the gas-liquid separation unit 6 by differential pressure can be stored in the storage container 200; Heating medium supply means for supplying and circulating the heating medium (HM) connected to the vaporization unit (1), the cooling unit (4), the water removal unit (5), the gas-liquid separation unit (6) and the transfer storage unit (7) class; a cooling medium supply means connected to the cooling unit 4, the water removal unit 5, the gas-liquid separation unit 6 and the transfer storage unit 7 to supply and circulate the cooling medium CM; a neutralization device for neutralizing and treating the water impurities discharged from each component; and a controller (not shown) that controls the overall operation of the system. As described above, dimethylamine is manufactured by reacting methanol and ammonia and sold as a liquid product. Due to the characteristics of the manufacturing process, the product includes not only dimethylamine, but also ammonia, moisture, monomethylamine, nitrogen, oxygen, and metal. It contains impurities such as, that is, dimethylamine is present in a low purity (about 95.5%) in the product, there is a problem that the product cannot be used for industrial purposes such as semiconductor processing. Accordingly, the present invention provides a system and method capable of producing dimethylamine of high purity (99.99%) by using a product containing dimethylamine in low purity as a raw material, that is, by removing impurities from the raw material. do.

The vaporizer 1 is configured to vaporize dimethylamine by applying heat to a raw material containing impurities and liquid dimethylamine under the control of the controller. ) located inside the raw material transfer tube 12 through which the raw material moves, and a separation unit 13 connected to the end of the raw material transfer tube 12 to remove liquid dimethylamine from the raw material discharged from the raw material transfer tube 12 and then discharge it ), and as the heating medium (eg, hot water, etc.) supplied from the heating medium supply device is supplied into the housing and flows around the raw material transfer tube 12, the raw material transfer tube 12 is heated to heat the inside. It is characterized in that the liquid dimethylamine is vaporized by allowing heat to be transferred to the flowing raw material.

The separation unit 13 has an upper side that communicates with the end of the raw material transfer tube 12, and is configured to remove liquid dimethylamine from the raw material discharged from the raw material transfer tube 12 and then discharge it. can be used The separation unit 13 may include a water level sensor (not shown) capable of measuring an internal water level.

Looking at the operation process of the vaporization unit 1 having the above configuration, helium gas is supplied to the raw material tank 100 of the tank lorry for raw material supply, and the raw material is transferred to the raw material transfer tube 12 at a pressure of about 2 to 2.5 bar. After supplying, when the heating medium supply device is operated to supply hot water at 34 to 40° C. to the housing 11, the raw material transfer tube 12 is heated and heat is transferred to the raw material flowing through the liquid dimethylamine After this is vaporized, the raw material discharged from the end of the raw material transfer tube 12 and introduced into the separation unit 13 is separated from the gas and liquid, and liquid dimethylamine is located on the lower side, and the liquid dimethyl amine is located on the lower side through the upper discharge tube 13a. Raw materials excluding the amine are discharged, and the liquid dimethylamine located at the lower side is sent to the neutralization facility through the discharge pipe 13b at the lower side. It is impossible to vaporize all of the liquid dimethylamine contained in the raw material, and when the liquid dimethylamine flows into the adsorption unit 2, the adsorption treatment efficiency decreases. The raw material from which dimethylamine has been removed is supplied to the adsorption unit 2 . In addition, the controller checks the level value of the liquid dimethylamine output from the water level sensor located inside the separation unit 13, and when it is determined that the predetermined level value is abnormal (for example, if the level of the separation unit is 15% or more), the raw material The raw material is not supplied from the tank 100 to the vaporization unit 1 to prevent liquid dimethylamine from being supplied to the adsorption unit 2 . The movement of the fluid in the manufacturing system, including the vaporization unit 1, is made by controlling a valve, a pump, etc. by a controller, which is a known matter irrelevant to the gist of the present invention, and thus a detailed description thereof will be omitted.

The adsorption unit 2 is configured to remove impurities by adsorbing the discharge of the vaporization unit containing impurities and gaseous dimethylamine under the control of the controller, and the adsorbent is loaded on the adsorption unit 2, As the adsorbent, at least one selected from the group consisting of Molecular sieve, activated carbon, and potassium hydroxide is used. It is preferable that a plurality of the adsorption unit 2 are formed in parallel, and it is preferable to maintain the surface temperature of the adsorption unit at 45 to 50° C. in order to prevent liquefaction according to the temperature/pressure deviation of dimethylamine, It is preferable to apply an explosion-proof heat tracing cable due to the characteristics of combustible gas. As the discharge of the vaporization unit 1 passes through the adsorption unit 2, ammonia is mainly removed, and some moisture is removed.

The specific gravity utilization processing unit 3 is configured to remove impurities from the discharge of the adsorption unit 2 by using the specific gravity difference under the control of the controller, and is a device for separating substances using the conventional gas specific gravity difference can be used The specific gravity utilization processing unit 3 includes a tower unit 31 in the form of a long tower, and when the discharge discharged from the adsorption unit 2 flows into the tower unit 31, the heavy material is located at the lower side and the light material is located on the upper side, that is, the discharge of the adsorption unit 2 is separated. Thereafter, the controller sequentially opens the upper pipe 32 installed at the upper end of the tower unit 31 and the side pipe 33 installed at the side so that the exhaust from which impurities are removed is supplied to the cooling unit 4 . . The discharge of the adsorption unit 2 includes gaseous dimethylamine, monomethylamine, nitrogen, oxygen, partially removed ammonia, partially removed moisture and metal, etc., and the discharge of the adsorption unit 2 uses the specific gravity. While passing through the processing unit 3, heavy metal, light nitrogen and oxygen are mainly removed. Light nitrogen and oxygen are discharged through the upper pipe 32 and sent to a neutralization facility, and heavy metal is sent to a reboiler to be described below.

The cooling unit 4 is configured to liquefy gaseous dimethylamine by cooling the discharge of the specific gravity utilization processing unit 3 under the control of the controller, and a conventional device such as a heat exchanger using a cooling medium may be used. . When the cooling unit 4 is operated, the controller operates the cooling medium supply device to supply the cooling medium at approximately -25°C and to maintain the recovery temperature of the cooling medium at -17°C, the pressure of liquid dimethylamine It is preferable to maintain about 0.3 bar. In addition, the cooling unit 4 is connected to a heating medium supply device (not shown), it is possible to remove the contaminants in the cooling unit 4 by receiving a heating medium when necessary.

The water removal unit 5 is configured to cool the discharge of the cooling unit 4 under the control of the controller to solidify the water to remove the water, and a discharge pipe through which the discharge of the cooling unit 4 moves ( 51), and a medium moving part 52 surrounding the exhaust pipe 51 and through which the cooling medium supplied from the cooling medium supply device flows. It is filled with a mesh plate or ceramic ball. The freezing point of water is 0°C, but in order to solidify and remove water in the state in which the flow path is formed, it must be maintained at a minimum of -20°C. It is preferable to supply the cooling medium at ℃ and to maintain the recovery temperature of the cooling medium at -25 DEG C, which is the cooling medium supply temperature condition of the cooling unit 4 . When the discharge of the cooling unit 4 passes through the discharge pipe 51 , the moisture is solidified by the cooling medium flowing through the medium moving unit 52 , and is fixed and separated in the discharge pipe 51 . Since a very small amount of water is contained in the discharge (the water contained in the raw material itself is small, and a certain amount of water has already been removed by the adsorption unit), even if the water is solidified and fixed in the discharge pipe 51, the flow of the discharge It is not affected, and the medium transfer unit 52 is connected to the heating medium supply device, so that it is possible to receive hot water when necessary, melt the ice in the discharge transfer tube 51 and remove it through the water discharge tube 53 . The present invention does not liquefy dimethylamine in the gas phase and remove moisture at once for the discharge of the specific gravity utilization treatment unit, but liquefy dimethylamine in the gas phase and then solidify and remove moisture in the next step to improve the impurity removal efficiency. there is.

The gas-liquid separation unit 6 separates the discharge of the water removal unit 5 into vapor phase impurities and liquid dimethylamine under the control of the controller, removes vapor phase impurities, and then heats and discharges liquid dimethylamine It is preferable that a plurality of pieces are formed in parallel to operate sequentially. The gas-liquid separation unit 6 includes a storage tank 61 for temporarily storing the discharge of the water removal unit 5, a jacket 62 surrounding the storage tank 61 and flowing a cooling medium or a heating medium, and the storage tank A vacuum pump 63 connected to the upper side of (62), a discharge pipe 64 connected to the lower end of the storage tank 61 for discharging dimethylamine, and a water level inside the storage tank 61 and a water level sensor (not shown) that can be measured.

Looking at the operation process of the gas-liquid separation unit 6, the controller operates the cooling medium supply device so that the cooling medium of approximately -30° C. flows through the jacket 62 to make the flow path smooth. The discharge of the removal unit 5 is supplied to the storage tank 61, and the controller checks the water level value output from the water level sensor and when it is determined that the predetermined water level value is abnormal (for example, if the level of the storage tank is 65% or more) , stop the inflow of the effluent and maintain it for a certain period of time (approximately 60 minutes) so that the effluent stored in the storage tank 61 is stabilized so that the light upper impurities (mainly nitrogen, hydrogen, monomethylamine, etc.) and the lower liquid phase Let it separate with dimethylamine. Then, the controller operates ^{the vacuum pump 63 to have a vacuum suction degree of 2.5×10 -2} torr or less to remove light upper impurities, and then operates the heating medium supply device to the jacket 62. By allowing a heating medium of approximately 35° C. to flow, heat is applied to the remaining liquid dimethylamine to vaporize it, and the pressure is raised to approximately 2 bar so that dimethylamine is discharged through the discharge pipe 64 by the pressure difference. Since a plurality of gas-liquid separation units 6 are installed in parallel, when the discharge is located at a certain water level in one gas-liquid separation unit, the discharge stops flowing into one gas-liquid separation unit, and the discharge flows into the other gas-liquid separation unit As a result, the processing capacity can be increased by sequentially using a plurality of gas-liquid separation units.

The transfer storage unit 7 is configured to cool the dimethylamine discharged from the gas-liquid separation unit 6 so that the dimethylamine discharged from the gas-liquid separation unit 6 by differential pressure can be stored in the storage container 200. , the dimethylamine discharged from the gas-liquid separation unit 6 has a high pressure, but the dimethylamine that has passed through the transfer storage unit 7 loses heat and has a low pressure, that is, a pressure difference occurs and is transferred without using a pump The liquid dimethylamine that has passed through the storage unit 7 may be stored in the storage container 200 . It may be considered to directly fill the storage container 200 with the liquid dimethylamine stored in the storage tank from which light impurities have been removed, using a pump. The present invention applies heat to liquid dimethylamine temporarily stored in a storage tank to increase the pressure, and cools the dimethylamine discharged to the storage tank in the process of passing through the transfer storage unit 7 to reduce the pressure, thereby reducing the pressure without using a pump. Dimethylamine from which light impurities are removed in the gas-liquid separation unit can be stored in the storage container. The transfer storage unit 7 includes a discharge pipe 71 through which the discharge of the gas-liquid separation unit 6 moves, and a cooling medium (approximately -15) that surrounds the discharge pipe 71 and is supplied from the cooling medium supply device. ℃) including a medium moving part 72 and the like through which it flows. The medium transfer unit 72 is connected to a heating medium supply device, and when necessary, it receives a heating medium of approximately 35° C. and recovers the dimethylamine remaining in the discharge tube 71, thereby preventing a safety accident due to liquid expansion. .

A high-purity dimethylamine manufacturing system according to another embodiment of the present invention has one end communicating with the lower end of the storage tank 61 and the other end communicating with the tower part 31 on the upper side of the side tube 33. Dimethylamine containing impurities above a certain level a first transport pipe 81 to be supplied to the tower part 31; One end communicates with the upper side of the storage container 200 and the other end communicates with the tower part 31 on the upper side of the side tube 33 so that the gaseous material of the storage container 200 is supplied to the tower part 31 . a transfer pipe 81; At the upper end, the tower part 31 communicates with the lower end, and a reboiler 83 that heats the dimethylamine supplied from the storage tank 61 or the gaseous material supplied from the storage container 200 to remove impurities by boiling. ) and the like. Impurities such as metals may be contained in the liquid dimethylamine separated from the storage tank 61 due to malfunction, etc., at a required level or more, and vaporized substances may be generated in the storage container 200 due to continuous use. The controller supplies the liquid dimethylamine of the storage tank 61 and/or the gaseous material of the storage container 200 to the tower part 31 through the first transfer pipe 81 and/or the second transfer pipe 82 and heats it. By operating the medium supply means, the heating medium is supplied to the reboiler 83 to heat the liquid dimethylamine or/and the gaseous material flowing into the tower, and the impurities in the gaseous phase are separated by the boiling point through the upper pipe 31 to be discharged, impurities such as metal are sent to the neutralization facility through the lower pipe (83a), and dimethylamine in the gas phase from which impurities are removed is discharged through the side pipe (33).

When a method for producing high-purity dimethylamine using a high-purity dimethylamine production system according to another embodiment of the present invention is described with reference to FIGS. 1 to 7, the method for producing the high-purity dimethylamine includes impurities and liquid dimethylamine. A vaporization step (S1) of vaporizing dimethylamine by applying heat to a raw material containing; an adsorption step (S2) of removing impurities by adsorbing the product of the vaporization step (S1) containing impurities and gaseous dimethylamine; a specific gravity utilization treatment step (S3) of removing impurities from the product of the adsorption step (S2) by using the specific gravity difference; a cooling step (S4) of cooling the product of the specific gravity utilization treatment step (S3) to liquefy the gaseous dimethylamine; a water removal step (S5) of cooling the product of the cooling step (S4) to solidify the water to remove the water; a gas-liquid separation step (S6) of separating the product of the water removal step (S5) into vapor phase impurities and liquid dimethylamine, removing the vapor phase impurities, and then discharging the liquid dimethylamine by heating; It includes a transfer and storage step (S7) of cooling the dimethylamine discharged in the gas-liquid separation step (6) so that the dimethylamine discharged in the gas-liquid separation step (S6) by the differential pressure can be stored in the storage container (200). .

The vaporization step (S1) is a step of vaporizing dimethylamine by applying heat to a raw material containing impurities and liquid dimethylamine, and heating the raw material containing impurities and liquid dimethylamine to vaporize dimethylamine; , and a separation step of removing dimethylamine in the liquid phase that has not been vaporized after the heating step.

The heating step is a step of heating a raw material containing impurities and liquid dimethylamine to vaporize dimethylamine. After the raw material is supplied to the raw material transfer tube 12 at a pressure of Heat is transferred to the flowing raw material to vaporize liquid dimethylamine.

The separation step is a step of removing the liquid dimethylamine that has not been vaporized after the heating step. In the separation step, the raw material discharged from the end of the raw material transfer tube 12 and introduced into the separation unit 13 is gas-liquid separated. , the liquid dimethylamine is located on the lower side, the raw materials except for the liquid dimethylamine are discharged through the upper discharge pipe (13a), and the liquid dimethylamine located on the lower side is transferred to the neutralization facility through the lower discharge pipe (13b). will be sent

The adsorption step (S2) is a step of removing impurities by adsorbing the product of the vaporization step (S1) containing impurities and gaseous dimethylamine, and in the adsorption step (S2), the product of the vaporization step (S1) While passing through the adsorption unit 2, ammonia is mainly removed, and some moisture is removed.

The specific gravity utilization treatment step (S3) is a step of removing impurities from the product of the adsorption step (S2) by using the specific gravity difference, and in the specific gravity utilization treatment step (S3), the product of the adsorption step (S2) is a tower The heavy material introduced into the part 31 is located at the lower side and the light material is located at the upper side, that is, the discharge of the adsorption step (S2) is separated, and light nitrogen and oxygen are discharged through the upper pipe 32 and neutralized It is sent to the facility, and the heavy metal is sent to the reboiler, which will be described below.

The cooling step (S4) is a step of cooling the product of the specific gravity utilization treatment step (S3) to liquefy the gaseous dimethylamine. In the cooling step (S4), the controller operates the cooling medium supply device, and approximately -25 A cooling medium of ℃ is supplied and the recovery temperature of the cooling medium is maintained at -17°C, so that the pressure of liquid dimethylamine is maintained at about 0.3 bar.

The water removal step (S5) is a step of removing water by cooling the product of the cooling step (S4) to solidify the water, and in the water removing step (S5), the product of the cooling step (S4) is the discharge pipe Passing through (51), the moisture is solidified by the cooling medium flowing through the medium transfer unit (52), and is fixed and separated in the discharge transfer tube (51).

The gas-liquid separation step (S6) is a step of separating the product of the water removal step (S5) into gaseous impurities and liquid dimethylamine, removing the gaseous impurities, and then discharging the liquid dimethylamine by applying heat. The inflow step of introducing the product of step (S5) into the storage tank, and when the product flows into the storage tank at a predetermined water level, the product is stopped and the product is left still for a certain period of time to obtain impurities in the upper gas phase and dimethylamine in the liquid phase at the bottom. It includes a separation step to separate into

The inflow step is a step of introducing the product of the water removal step (S5) into the storage tank. In the introduction step (S4), the controller operates the cooling medium supply device to the jacket 62 surrounding the storage tank 61. The product of the water removal step (S5) is supplied to the storage tank 61 in a state in which the flow path is smoothed by allowing the cooling medium of -30°C to flow.

In the separation step, when the product is introduced into the storage tank at a certain level, the product is stopped and the product is left still for a certain period of time so as to be separated into impurities in the gas phase at the upper side and dimethylamine in the liquid phase at the bottom, in the separation step When the controller checks the water level value output from the water level sensor and determines that the predetermined water level value is abnormal (for example, if the level of the storage tank is 65% or higher), it stops the inflow of the discharge and maintains a predetermined time (approximately 60 minutes). The discharge stored in the storage tank 61 is stabilized so that it is separated into light impurities (mainly nitrogen, hydrogen, monomethylamine, etc.) on the upper side and dimethylamine in the liquid phase on the lower side.

The gaseous impurities removing step is a step of removing impurities in the gaseous phase after the separation step. In the gaseous impurities removing step, the vacuum pump 63 is operated so that the ^{controller has a vacuum suction degree of 2.5×10 −2 torr or less.} Allow the light upper impurities to be removed.

The boosting step is a step of increasing the pressure by applying heat to the liquid dimethylamine after the gaseous impurity removal step. Heat is applied to the remaining liquid dimethylamine to flow, and the pressure is raised to approximately 2 bar, so that dimethylamine is discharged through the discharge pipe 64 by the pressure difference.

The transfer and storage step (S7) is a step of cooling the dimethylamine discharged from the gas-liquid separation step (6) so that the dimethylamine discharged from the gas-liquid separation step (S6) can be stored in the storage container 200 by the differential pressure. , in the transfer storage step, the dimethylamine discharged to the storage tank is cooled in the process of passing through the transfer storage unit 7 to reduce the pressure, so that dimethyl amine from which light impurities are removed from the gas-liquid separation unit without using a pump It is possible to store the amine in the storage container.

In the method for producing high-purity dimethylamine according to another embodiment of the present invention, the dimethylamine supplied from the storage tank 61 or the gaseous material supplied from the storage container 200 is heated to remove impurities by boiling point and then discharged. It may further include a boiling point separation step, the product of the boiling point separation step is sent to the cooling unit.

Hereinafter, the present invention will be described in more detail through examples. However, these are only for describing the present invention in more detail, and the scope of the present invention is not limited thereto.

<Example 1> Construction of manufacturing system and setting of operating conditions

1. A manufacturing system as shown in FIG. 1 was constructed, and an adsorbent in which Morecuresib and potassium hydroxide were mixed was used.

2. Supplying helium gas at a pressure of 2.5 bar to the raw material tank 100, supplying hot water at 37° C. to the vaporization unit 1, and causing the surface temperature of the adsorption unit 2 to be 45° C. or higher, A cooling medium of -25° C. is supplied to the cooling unit 4 so that the recovery temperature of the cooling medium is maintained at -17° C., a cooling medium of -30° C. is supplied to the water removal unit 5, and the recovery temperature of the cooling medium. is maintained at -25 ° C, and a cooling medium of -30 ° C flows through the jacket 62, and when the level of the reservoir is 65% or higher, stop the inflow of the discharge and hold for 60 minutes, 2.5 × 10 ^{- The} vacuum pump was operated to have a vacuum suction degree of 2 torr or less, and then a heating medium of about 35° C. was flowed through the jacket 62, and the remaining liquid dimethylamine was heated and vaporized to raise the pressure to about 2 bar. , a cooling medium of -15°C was supplied to the transfer storage unit (7).

<Example 2> Preparation of high-purity dimethylamine using a manufacturing system

1. According to the production system and operating conditions of Example 1, the raw material was purified to prepare high-purity dimethylamine. Specifically, the raw material was supplied to the vaporizer to vaporize dimethylamine, and the liquid dimethylamine was removed from the vaporizer to be supplied to the adsorption unit. After that, the discharge from the vaporization unit passes through the adsorption unit to remove impurities, the discharge from the adsorption unit passes through the specific gravity utilization treatment unit to remove impurities, and the discharge from the specific gravity utilization treatment unit passes through the cooling unit to liquefy gaseous dimethylamine , the exhaust from the cooling unit passed through the water removal unit to remove moisture. In addition, the discharge of the water removal unit passed through the gas-liquid separation unit to be separated into vapor phase impurities and liquid dimethylamine, and then vapor phase impurities were removed, and the liquid dimethylamine was heated to increase the pressure. Thereafter, the discharge from the gas-liquid separation unit passed through the transfer storage unit to cool the dimethylamine, and the dimethylamine was filled in the storage container by the differential pressure to prepare high-purity dimethylamine.

2. The components of the raw material, the adsorption unit discharge, the cooling unit discharge, the water removal unit discharge, and the gas-liquid separation unit discharge during the manufacturing process of Example 2 were analyzed and shown in Table 1 below. In Table 1, "-" indicates that the concentration of a specific component is not measured.

3. Referring to Table 1, it can be seen that dimethylamine of high purity (99.99%) can be obtained using the manufacturing system, ammonia and moisture are removed from the adsorption unit, and nitrogen and hydrogen are removed from the specific gravity utilization treatment unit. , it can be seen that moisture is removed from the water removal unit, and nitrogen, hydrogen, and monomethylamine can be effectively removed from the gas-liquid separation unit.

ingredient Raw material adsorption unit
emissions cooling unit
emissions moisture removal unit
emissions gas-liquid separator
emissions (CH ₃ ) ₂ NH (%) 99.5 - - - 99.99 N ₂ (ppmv) <1,000 - <170 - <10 O ₂ (ppmv) <50 - <30 - <5 NH ₃ (ppmv) <30 <2 <5 - <3 H ₂ O (ppmv) <100 <20 <20 <5 <5 CH ₃ NH ₂ (ppmv) <50 <50 <50 - <5

In the above, the applicant has described preferred embodiments of the present invention, but these embodiments are only one embodiment that implements the technical idea of the present invention, and any changes or modifications as long as the technical idea of the present invention is implemented. should be construed as within the scope.

1: vaporization unit 2: adsorption unit 3: specific gravity utilization treatment unit
4: Cooling unit 5: Water removal unit 6: Gas phase separation unit
7: transfer storage unit 11: housing 12: raw material transfer tube
13: separation part 13a, 13b: discharge pipe 31: tower part
32: upper pipe 33: side pipe 51, 71: discharge pipe
52: 72: medium transfer unit 53: water discharge pipe 61: storage tank
62: jacket 63: vacuum pump 64: exhaust pipe
81: first transfer tube 82: second transfer tube 83: reboiler
83a: lower pipe 100: raw material tank 200: storage container

Claims (8)

a vaporizer for vaporizing dimethylamine by applying heat to a raw material containing impurities and liquid dimethylamine; an adsorption unit for removing impurities by adsorbing the waste product of the vaporization unit containing impurities and gaseous dimethylamine; a specific gravity utilization processing unit for removing impurities from the discharge of the adsorption unit by using the specific gravity difference; a cooling unit for cooling the discharge of the specific gravity utilization processing unit to liquefy dimethylamine in the gas phase; and a water removal unit for removing water by cooling the discharge of the cooling unit to solidify water.
The impurities are ammonia, moisture, monomethylamine, high-purity dimethylamine production system, characterized in that it includes nitrogen and oxygen. According to claim 1,
The high-purity dimethylamine manufacturing system includes: a gas-liquid separation unit for separating the discharge of the water removal unit into vapor phase impurities and liquid dimethylamine, removing vapor phase impurities, and then discharging liquid dimethylamine by heating; A high-purity dimethylamine manufacturing system comprising a; a transfer storage unit for cooling the dimethylamine discharged from the gas-liquid separation unit so that the dimethylamine discharged from the gas-liquid separation unit by the differential pressure can be stored in the storage container. 3. The method of claim 2,
The vaporization unit includes a housing forming an outer shape, a raw material transfer tube located inside the housing and through which the raw material moves, and a separation unit that is connected to the end of the raw material transfer tube to remove liquid dimethylamine from the raw material discharged from the raw material transfer tube and then discharges it. Including, as the heating medium supplied from the heating medium supply device is supplied into the housing and flows around the raw material transfer tube, the raw material transfer tube is heated to transfer heat to the raw material flowing inside, thereby vaporizing liquid dimethylamine make it,
The raw material discharged from the end of the raw material transfer tube and introduced into the separation unit is separated from gas and liquid, liquid dimethylamine is located on the lower side, and the controller discharges the raw material except for liquid dimethylamine through the upper discharge tube, located on the lower side A high-purity dimethylamine manufacturing system, characterized in that the liquid dimethylamine is sent to the neutralization facility through the lower discharge pipe. 4. The method of claim 3,
The controller checks the level value of the liquid dimethylamine output from the water level sensor located inside the separation unit. If it is determined that the predetermined level value is abnormal, the raw material is not supplied to the vaporization unit, and the liquid dimethylamine is supplied to the adsorption unit. A high-purity dimethylamine production system, characterized in that it prevents it from becoming. 5. The method of claim 4,
The adsorbent is loaded with an adsorbent, and any one or more selected from the group consisting of morecuresib, activated carbon and potassium hydroxide is used as the adsorbent,
A high-purity dimethylamine production system, characterized in that ammonia is removed while the discharge of the vaporization unit passes through the adsorption unit. 6. The method of claim 5,
The specific gravity utilization processing unit includes a tower in the form of a long tower, and when the discharge discharged from the adsorption unit flows into the tower unit, the heavy material is located at the lower side and the light material is located at the upper side, so that the discharge of the adsorption unit is separated,
High-purity dimethylamine production system, characterized in that light nitrogen and oxygen are removed while the discharge of the adsorption unit passes through the specific gravity utilization treatment unit. 7. The method of claim 6,
The gas-liquid separation unit includes a storage tank for temporarily storing the discharge of the water removal unit, a jacket surrounding the storage tank and flowing a cooling medium or a heating medium, a vacuum pump connected to an upper side of the storage tank, and a lower end of the storage tank. It includes a discharge pipe for discharging the amine, and a water level sensor located inside the storage tank to measure the water level inside,
The controller operates the cooling medium supply device to allow the cooling medium to flow through the jacket so that the discharge of the water removal unit is supplied to the storage tank while the flow path is smoothed;
The controller checks the water level value output from the water level sensor and, if it is determined that the predetermined water level value is abnormal, stops the inflow of the discharge and maintains a predetermined time to stabilize the discharge stored in the storage tank. to be separated with dimethylamine,
The controller operates the vacuum pump to remove light upper impurities, operates the heating medium supply device to allow the heating medium to flow through the jacket, and applies heat to the remaining liquid dimethylamine to vaporize it and increase the pressure to increase the pressure difference A high-purity dimethylamine production system, characterized in that the dimethylamine is discharged through the discharge pipe by the 8. The method of claim 7,
The dimethylamine discharged from the gas-liquid separation unit has high pressure, but the dimethylamine that has passed through the transfer storage unit loses heat and has a low pressure, resulting in a pressure difference, so that the liquid dimethylamine passed through the transfer storage unit without using a pump A high-purity dimethylamine production system, characterized in that it can be stored in a storage container.

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