CN218451884U - Thiourea-based propionic acid crystallization system - Google Patents

Thiourea-based propionic acid crystallization system Download PDF

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CN218451884U
CN218451884U CN202222310977.6U CN202222310977U CN218451884U CN 218451884 U CN218451884 U CN 218451884U CN 202222310977 U CN202222310977 U CN 202222310977U CN 218451884 U CN218451884 U CN 218451884U
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mother liquor
addition
propionic acid
thioureido
cauldron
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于志红
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Ningxia Xinrui Biotechnology Co ltd
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Ningxia Xinrui Biotechnology Co ltd
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Abstract

The utility model provides a thioureido propionic acid crystal system is including holding elevated tank, addition cauldron, crystallization kettle, centrifuge, mother liquor jar, the effluent water sump of acrylic acid, the addition cauldron is equipped with first feed inlet, second feed inlet, the elevated tank passes through the pipeline intercommunication with the first feed inlet of addition cauldron, and acrylic acid gets into the addition cauldron from the elevated tank, and thiourea, hydrochloric acid, water get into the addition cauldron from the second feed inlet, the discharge gate of addition cauldron passes through the pipeline intercommunication with crystallization kettle's feed inlet, and crystallization kettle's discharge gate passes through the pipeline intercommunication with centrifuge's feed inlet to with thioureido propionic acid crystal and mother liquor separation, centrifuge still is equipped with the water inlet to the washing crystal, centrifuge's liquid outlet passes through the pipeline intercommunication with the inlet of mother liquor jar, the liquid outlet of mother liquor jar and crystallization kettle's feed inlet intercommunication are in order to let in the mother liquor into crystallization kettle.

Description

Thiourea-based propionic acid crystallization system
Technical Field
The utility model relates to a chemical industry technical field especially relates to a thioureido propionic acid crystal system.
Background
Thioureidopropionic acid is an intermediate of the pharmaceutical fenamic acid and is also used as a stabilizer for polyvinyl chloride. It can be used in transparent products like thioglycolic acid, and has good thermal stability, superior to other stabilizers. Also useful as antioxidants, catalysts and biochemicals. One method for preparing the thioureido propionic acid is to obtain liquid thioureido propionic acid by addition reaction of thiourea, acrylic acid and hydrochloric acid. And the liquid thiourea propionic acid is separated by a centrifuge after being crystallized, and the mother liquor enters a sewage treatment tank for treatment. Since the mother liquor still contains a small amount of thioureido propionic acid, the yield of the thioureido propionic acid is influenced in the past.
Disclosure of Invention
In view of the above, it is necessary to provide a thioureido propionic acid crystallization system which can improve the yield of thioureido propionic acid.
The utility model provides a thioureido propionic acid crystal system is including holding the elevated tank, addition cauldron, crystallization kettle, centrifuge, mother liquor jar, effluent water sump of acrylic acid, the addition cauldron is equipped with first feed inlet, second feed inlet, the elevated tank passes through the pipeline intercommunication with the first feed inlet of addition cauldron, and acrylic acid gets into the addition cauldron from the elevated tank, and thiourea, hydrochloric acid, water get into the addition cauldron from the second feed inlet, the discharge gate of addition cauldron passes through the pipeline intercommunication with crystallization kettle's feed inlet, and crystallization kettle's discharge gate passes through the pipeline intercommunication with centrifuge's feed inlet to with thioureido propionic acid crystal and mother liquor separation, centrifuge still is equipped with the water inlet to the washing crystal, centrifuge's liquid outlet and the inlet of mother liquor jar pass through the pipeline intercommunication, the liquid outlet of mother liquor jar and crystallization kettle's feed inlet intercommunication to let in the crystallization kettle with the mother liquor.
Preferably, the liquid outlet of the mother liquid tank is also communicated with a pipeline of the addition kettle through a pipeline so as to dilute the materials in the addition kettle.
Preferably, the mother liquor tank still includes pH sensor, controller, two control valves, the pH sensor sets up in the mother liquor tank to detect the pH value of the mother liquor in the mother liquor tank, including pH sensor and controller electric connection, the controller still with control valve electric connection, one of them control valve sets up on the pipeline between mother liquor tank and the addition cauldron, the liquid outlet of mother liquor tank still passes through the pipe connection with external sewage treatment pond, another control valve sets up on the pipeline between mother liquor tank and sewage treatment pond.
Preferably, the addition kettle is also provided with a steam interlayer, and steam is introduced into the steam interlayer to heat the materials in the addition kettle so as to generate the thioureido propionic acid.
Preferably, the crystallization kettle is provided with a frozen brine interlayer, and the frozen brine interlayer is filled with frozen brine for cooling.
Has the advantages that: the utility model discloses a thioureido propionic acid crystal system is through the liquid outlet with the mother liquor jar and the feed inlet intercommunication of crystallization kettle for during the mother liquor enters into thioureido propionic acid solution, the small crystalline grain that contains in the mother liquor provides the crystal nucleus for thioureido propionic acid solution, can accelerate thioureido propionic acid and form the crystallization, and the thioureido propionic acid of dissolving state can make the thioureido propionic acid solution among the crystallization kettle form supersaturated solution in the on the other hand mother liquor, thereby accelerates the crystallization of thioureido propionic acid. On the other hand, the crystallization kettle utilizes the thioureido propionic acid in the mother solution, so that the yield of the thioureido propionic acid is improved.
Drawings
FIG. 1 is a process flow diagram of the thioureido propionic acid crystallization system of the present invention.
In the figure: elevated tank 1, addition kettle 2, steam interlayer 201, second feed inlet, crystallization kettle 3, frozen brine interlayer 301, centrifuge 4, mother liquor tank 5, control valve 501 and sewage pool 6.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
Referring to fig. 1, a thioureido propionic acid crystallization system comprises an elevated tank 1 for containing acrylic acid, an addition kettle 2, a crystallization kettle 3, a centrifuge 4, a mother liquor tank 5 and a sewage tank 6, wherein the addition kettle 2 is provided with a first feed port and a second feed port, an outlet of the elevated tank 1 is communicated with the first feed port of the addition kettle 2 through a pipeline, acrylic acid enters the addition kettle 2 from the elevated tank 1, thiourea, hydrochloric acid and water enter the addition kettle 2 from the second feed port, a discharge port of the addition kettle 2 is communicated with a feed port of the crystallization kettle 3 through a pipeline, a discharge port of the crystallization kettle 3 is communicated with a feed port of the centrifuge 4 through a pipeline to separate thioureido propionic acid crystals from the mother liquor, the centrifuge 4 is further provided with a water inlet to clean the crystals, a liquid outlet of the centrifuge 4 is communicated with a liquid inlet of the mother liquor tank 5 through a pipeline, and a liquid outlet of the mother liquor tank 5 is communicated with a feed port of the crystallization kettle 3 to introduce the mother liquor into the crystallization kettle 3.
The utility model discloses a thioureido propionic acid crystal system is when the operation, and acrylic acid, thiourea react in addition cauldron 2 under hydrochloric acid environment and the uniform temperature condition, generate and use thioureido propionic acid as the main part to the mixed solution of a small amount of acrylic acid, thiourea, hydrochloric acid in addition. The mixed solution is fed from the addition vessel 2 to the crystallization vessel 3. Under a certain temperature condition, the thioureido propionic acid in the mixed solution forms crystals, and the mixed solution becomes a solid-liquid mixture. The solid-liquid mixture enters a centrifuge 4 from a crystallization kettle 3. Under the action of the centrifuge 4, the liquid is separated to become mother liquid, and the thiourea propionic acid solid is cleaned and then is centrifugally separated again to enter the next link. The mother liquor discharged from the centrifuge 4 enters the crystallization kettle 3, and the thiourea-based propionic acid in a dissolved state in the mother liquor can enable the thiourea-based propionic acid solution in the crystallization kettle 3 to form a supersaturated solution. Meanwhile, a certain amount of thioureido propionic acid crystals are added into the crystallization kettle 3 to be used as seed crystals, so that precipitated thioureido propionic acid can grow on the surface of the seed crystals, the wall-hanging phenomenon of the thioureido propionic acid crystals is eliminated, and good crystals are formed. The good crystal form is beneficial to reducing the load of a subsequent centrifuge, simultaneously improves the yield of the product and reduces the loss of materials in the mother liquor.
The utility model discloses an addition reaction primary reaction of thioureido propionic acid takes place addition reaction for the thiourea and generates beta-thioureido propionic acid (3-thioureido propionic acid) on acrylic acid beta-carbon, and the byproduct reaction takes place addition reaction for the thiourea and generates alpha-thioureido propionic acid (2-thioureido propionic acid) on acrylic acid alpha-carbon, and addition reaction accomplishes in addition cauldron 2.
Further, the liquid outlet of the mother liquor tank 5 is communicated with the pipeline of the addition kettle 2, the mother liquor enters the addition kettle 2, a steam interlayer 201 is arranged in the addition kettle 2, thiourea, hydrochloric acid and water enter the addition kettle 2 from a second feed inlet, the steam interlayer 201 heats the mother liquor in the addition kettle 2, and the mother liquor still contains a small amount of non-crystallized thioureido propionic acid, thiourea and hydrochloric acid and has lower concentration, so that the materials in the addition kettle 2 can be diluted.
Mother liquor tank 5 still includes pH sensor, controller, control valve 501, the pH sensor sets up in mother liquor tank 5 to detect the pH value of the mother liquor in mother liquor tank 5, including pH sensor and controller electric connection, the controller still with control valve 501 electric connection, one of them control valve 501 sets up on mother liquor tank 5 and the pipeline between addition cauldron 2, the liquid outlet of mother liquor tank 5 still passes through the pipe connection with external sewage treatment pond 6, another control valve 501 sets up on the pipeline between mother liquor tank 5 and sewage treatment pond 6.
After the materials in the crystallization kettle 3 are crystallized, the materials become a solid-liquid mixture, after the materials are acted by the centrifuge 4, the liquid part becomes mother liquor and enters the mother liquor tank 5, and the mother liquor of the part contains a small amount of tiny thioureido propionic acid crystals which can enter the crystallization kettle 3 to promote crystallization. Meanwhile, the mother liquor of the part also contains thiourea and hydrochloric acid with lower concentration, and can also be used as diluent to enter the addition kettle 2 to participate in addition reaction. The crystals in centrifuge 4 also require washing of the surface with residual mother liquor by water. The cleaned water then enters the mother liquor tank 5 by centrifugation. The liquid concentration of the part is unstable, and the hydrogen ion concentration in the liquid needs to be detected by a pH sensor, and how to treat the part of the liquid is judged according to the hydrogen ion concentration.
Specifically, the pH sensor detects the concentration of hydrogen ions in the liquid and transmits the concentration to the controller, the controller generates a real-time hydrogen ion concentration value, the controller is also provided with a hydrogen ion concentration reference value, and when the real-time hydrogen ion concentration value is larger than the hydrogen ion concentration reference value, a control valve on a pipeline between the mother liquor tank 5 and the addition kettle 2 is opened to enable the liquid to enter the addition kettle 2; when the real-time hydrogen ion concentration value is smaller than the hydrogen ion concentration reference value, a control valve 501 on a pipeline between the mother liquor tank 5 and the sewage treatment tank 6 is opened, so that the liquid enters the sewage treatment tank 6.
In a preferred embodiment, the addition reactor 2 is further provided with a steam interlayer 201, and steam is introduced into the steam interlayer 201 to heat the material in the addition reactor 2, so as to generate thioureido propionic acid.
In a preferred embodiment, the crystallization kettle 3 is provided with a frozen brine interlayer 301, and the frozen brine interlayer 301 is filled with frozen brine for cooling.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.

Claims (5)

1. A thioureido propionic acid crystallization system, characterized by: including overhead tank, addition cauldron, crystallization kettle, centrifuge, mother liquor jar that hold acrylic acid, the addition cauldron is equipped with first feed inlet, second feed inlet, the overhead tank passes through the pipeline intercommunication with the first feed inlet of addition cauldron, and acrylic acid gets into the addition cauldron from the overhead tank, and thiourea, hydrochloric acid, water get into the addition cauldron from the second feed inlet, the discharge gate of addition cauldron passes through the pipeline intercommunication with the feed inlet of crystallization kettle, and the discharge gate of crystallization kettle passes through the pipeline intercommunication with the feed inlet of centrifuge to with thioureido propionic acid crystal and mother liquor separation, centrifuge still is equipped with the water inlet to the washing crystal, centrifuge's liquid outlet and the inlet of mother liquor jar pass through the pipeline intercommunication, the liquid outlet of mother liquor jar and the feed inlet intercommunication of crystallization kettle to let in the crystallization kettle with the mother liquor.
2. A thioureido propionic acid crystallization system, as claimed in claim 1, wherein: and a liquid outlet of the mother liquid tank is also communicated with a pipeline of the addition kettle through a pipeline so as to dilute the materials in the addition kettle.
3. The thioureido propionic acid crystallization system of claim 1 wherein: mother liquor tank still includes pH sensor, controller, two control valves, the pH sensor sets up in the mother liquor tank to detect the pH value of the mother liquor in the mother liquor tank, including pH sensor and controller electric connection, the controller still with control valve electric connection, one of them control valve sets up on the pipeline between mother liquor tank and the addition cauldron, the liquid outlet of mother liquor tank still passes through the pipe connection with external sewage treatment pond, another control valve setting is on the pipeline between mother liquor tank and sewage treatment pond.
4. The thioureido propionic acid crystallization system of claim 1 wherein: the addition kettle is also provided with a steam interlayer, and steam is introduced into the steam interlayer to heat the materials in the addition kettle so as to generate the thioureido propionic acid.
5. The thioureido propionic acid crystallization system of claim 1 wherein: the crystallization kettle is provided with a frozen brine interlayer, and frozen brine is introduced into the frozen brine interlayer to cool.
CN202222310977.6U 2022-08-31 2022-08-31 Thiourea-based propionic acid crystallization system Active CN218451884U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118079823A (en) * 2024-04-18 2024-05-28 东营新航新材料科技有限公司 Thiourea synthesis system and method for preparing thiourea

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118079823A (en) * 2024-04-18 2024-05-28 东营新航新材料科技有限公司 Thiourea synthesis system and method for preparing thiourea

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