CN211099033U - Dicyandiamide recovery plant in glycocyamine production process - Google Patents

Dicyandiamide recovery plant in glycocyamine production process Download PDF

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CN211099033U
CN211099033U CN201921881600.8U CN201921881600U CN211099033U CN 211099033 U CN211099033 U CN 211099033U CN 201921881600 U CN201921881600 U CN 201921881600U CN 211099033 U CN211099033 U CN 211099033U
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kettle
dicyandiamide
cooling
impurity removing
kettles
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杨立彬
刘伟国
沈承琪
张文霞
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Beijing Junde Tongchuang Biotechnology Co ltd
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Beijing Junde Tongchuang Biotechnology Co ltd
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Abstract

The utility model provides dicyandiamide recovery equipment in a glycocyamine production process, which comprises an impurity removal kettle, a cooling kettle and a filter, wherein the impurity removal kettle is arranged at the upstream of the equipment, the impurity removal kettle comprises a plurality of impurity removal kettles, the impurity removal kettles are respectively connected with the cooling kettle, a condenser is also arranged on each impurity removal kettle, the condenser is vertically arranged on the impurity removal kettle, and the bottom end of the condenser is connected with the upper end of the impurity removal kettle through a connecting pipe; the cooling kettles are arranged at the downstream of the impurity removal kettles and are used for cooling and separating out dicyandiamide crystals; the filter is arranged at the downstream of the cooling kettle and is used for filtering the separated dicyandiamide crystals. The utility model provides a dicyandiamide recovery plant for in glycocyamine production process to ensure the cyclic utilization number of times of mother liquor, improve the utilization ratio to dicyandiamide simultaneously.

Description

Dicyandiamide recovery plant in glycocyamine production process
Technical Field
The invention relates to chemical equipment, in particular to dicyandiamide recycling equipment used in a glycocyamine production process.
Background
Guanidinoacetic acid (guanidineacetic acid), also known as guanidinoacetic acid, belongs to amino acids and derivatives thereof, is a functional feed, and is suitable for livestock and poultry mainly based on plant daily ration. The use of the glycocyamine has important significance for improving the production performance of livestock and poultry organisms, improving the meat quality, improving the resource value of protein feed and the like.
① guanidine hydrochloride, chloroacetic acid and sodium hydroxide are used as main raw materials, firstly guanidine hydrochloride and sodium hydroxide react at a certain temperature to generate free guanidine, then the generated free guanidine, chloroacetic acid and sodium hydroxide react at a certain temperature to generate guanidinoacetic acid, a certain reaction time is kept, a reaction product is filtered, dried and crushed after the reaction is completed to obtain a finished product, ② cyanamide, glycine and sodium hydroxide are used as main raw materials, firstly, glycine and sodium hydroxide are dissolved in water, and a cyanamide solution is dripped at a certain temperature to react to generate a crude guanidinoacetic acid product, and the product is obtained after the reaction is completed and the product is refined, filtered and dried.
Since chloroacetic acid belongs to dangerous chemicals, and the process steps for synthesizing glycocyamine by taking chloroacetic acid as a raw material are more, and the operation is complex, the process for synthesizing glycocyamine by taking cyanamide and glycine as raw materials is frequently used at present. The process has the advantages of simple operation, mild synthesis conditions and high product purity. However, the dicyandiamide in the raw material is easy to polymerize to form dicyandiamide, so that the recovery of dicyandiamide in the mother liquor can purify the mother liquor and increase the cycle number of the mother liquor, and the dicyandiamide as a medical intermediate also has certain economic value.
At present, no relevant equipment for recovering dicyandiamide in the production process of glycocyamine exists in China, so that dicyandiamide recovery equipment for the production process of glycocyamine is needed to ensure the recycling frequency of mother liquor and improve the utilization rate of dicyandiamide.
SUMMERY OF THE UTILITY MODEL
In view of the above problem, the utility model aims at providing a dicyandiamide recovery plant for in glycocyamine production process through setting up a plurality of edulcoration cauldron, cooling kettle and filter, with the dicyandiamide that exists in the mother liquor in the glycocyamine production process in addition recycle, improves the cycle number of mother liquor simultaneously.
The utility model provides a technical scheme that above-mentioned technical problem adopted is:
the improvement of dicyandiamide recovery equipment in the production process of glycocyamine is that the equipment comprises an impurity removal kettle, a cooling kettle and a filter, wherein,
the impurity removing kettles are arranged at the upstream of the equipment, the impurity removing kettles comprise a plurality of impurity removing kettles, the impurity removing kettles are respectively connected with the cooling kettle, a condenser is also arranged on each impurity removing kettle, the condenser is vertically arranged on the impurity removing kettles, and the bottom ends of the condensers are connected with the upper ends of the impurity removing kettles through connecting pipes;
the cooling kettles are arranged at the downstream of the impurity removal kettles and are used for cooling and separating out dicyandiamide crystals;
the filter is arranged at the downstream of the cooling kettle and is used for filtering the separated dicyandiamide crystals.
Further, in the dicyandiamide recovery plant in the glycocyamine production process, the number of the impurity removal kettles is 2, the impurity removal kettles are cylindrical closed containers, a stirring motor is arranged at the top end of each impurity removal kettle, and a stirring paddle connected with the stirring motor through a stirring rod is arranged inside each impurity removal kettle.
Further, in the dicyandiamide recovery equipment in the production process of glycocyamine, the stirring paddle comprises an upper layer paddle and a lower layer paddle, the upper layer paddle is provided with three blades, the upward inclination angle of each blade is 30-35 degrees, the lower layer paddle is provided with three blades, and each blade is inclined upwards by 30-35 degrees.
Further, in the dicyandiamide recovery equipment in the production process of glycocyamine, a heating jacket is arranged on the outer wall of the impurity removal kettle, a mother liquor inlet for injecting mother liquor is arranged at the top end of the impurity removal kettle, and a catalyst inlet and a temperature monitor are arranged on the side wall of the impurity removal kettle.
Further, in the dicyandiamide recovery plant in the production process of glycocyamine, the cooling kettle is a cylindrical closed container, the top end of the cooling kettle is provided with a stirring motor, and a stirring paddle connected with the stirring motor through a stirring rod is arranged in the cooling kettle.
Further, in the dicyandiamide recovery equipment in the production process of glycocyamine, the stirring paddle comprises an upper layer paddle and a lower layer paddle, the upper layer paddle is provided with three blades, the upward inclination angle of each blade is 30-40 degrees, the lower layer paddle is provided with three blades, and each blade is inclined upwards by 30-40 degrees.
Further, in the dicyandiamide recycling equipment in the production process of glycocyamine, a cooling jacket is arranged on the outer wall of the cooling kettle, a sampling window is arranged at the top end of the cooling kettle, a cooling inlet is arranged at the bottom end of the side wall of the cooling kettle, and a cooling outlet is arranged at the top end of the side wall of the cooling kettle.
Further, in the dicyandiamide recovery equipment in the production process of glycocyamine, the filter is designed in a closed manner, a filter tank is arranged in the filter, and filter cloth is filled in the filter tank and used for filtering dicyandiamide crystals.
Further, in the above dicyandiamide recovery apparatus in a glycocyamine production process, the top end of the filter is provided with a compressed air inlet for passing compressed air.
Further, in the above dicyandiamide recovery apparatus in a glycocyamine production process, the compressed air inlet is provided in plurality.
The utility model has the advantages that: the utility model discloses a set up two edulcoration kettles and carry out the edulcoration with the mother liquor in the guanidoacetic acid production process, the mother liquor after will decontaminating cools off through the cooling kettle, separates out the dicyandiamide in the mother liquor, filters back filtering dicyandiamide and continues recycle with the mother liquor of filtering dicyandiamide through the filter with the mother liquor of the dicyandiamide crystal that separates out. Simultaneously, for collecting the ammonia that the mother liquor edulcoration in-process produced, the utility model discloses still be provided with the condenser in edulcoration cauldron upper end, the mother liquor can produce the ammonia at the edulcoration in-process, and the ammonia is heated and upwards volatilizees, opens the valve of condenser this moment, and the ammonia gets into behind the condenser condensation and gets rid of for the aqueous ammonia, avoids the atmospheric pressure in the edulcoration cauldron too big, also avoids remaining the ammonia in the mother liquor after the edulcoration simultaneously. For ensuring mother liquor edulcoration efficiency, the utility model discloses still set up agitator motor drive stirring rake on the edulcoration cauldron and mix the mixture that the mother liquor accelerated mother liquor and catalyst, improve catalytic efficiency simultaneously. And a heating jacket is arranged on the outer wall of the impurity removal kettle to improve the activity of the catalyst. And set up temperature monitor at the edulcoration cauldron outer wall, constantly monitor the temperature in the edulcoration cauldron, ensure real-time efficient edulcoration. Still through setting up the sample window on the cooling kettle, make things convenient for operating personnel to take a sample at any time, look over the dicyandiamide in the mother liquor and precipitate the condition, avoid precipitating inadequately abundant. Compressed air inlet is arranged at the upper end of the filter, and compressed air is introduced into the filter, so that the filtering efficiency of dicyandiamide is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the technical solutions in the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a three-dimensional structure diagram of the present invention.
Wherein: 1-impurity removing kettle; 11-heating jacket; 12-a temperature monitor; 13-catalyst inlet; 14-a first valve; 15-mother liquor inlet; 2-cooling the kettle; 21-a sampling window; 22-cooling inlet; 23-a cooling outlet; 24-a second valve; 3-a filter; 31-a filter tank; 32-filter cloth; 33-compressed air inlet; 34-mother liquor recovery port; 35-a third valve; 4-a condenser; 41-water outlet; 42-a water inlet; 43-safety valve; 44-a liquid ammonia recovery port; 51-a stirring motor; 52-a stirring rod; 53-blade.
Detailed Description
The technical solution of the present invention will be described clearly and completely with reference to the accompanying drawings, and obviously, the described embodiments are some, but not all embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
As shown in fig. 1, fig. 1 is a three-dimensional structure diagram of the present invention. The utility model discloses a accessory substance in mother liquor in the production process of glycocyamine, namely the recovery plant of dicyandiamide, this equipment includes: edulcoration cauldron 1, cooling kettle 2, filter 3 and condenser 4, wherein, the most upper reaches of equipment are located to edulcoration cauldron 1 for carry out the edulcoration to the mother liquor in the glycocyamine production process, the lower extreme of edulcoration cauldron 1 is connected with cooling kettle 2's upper end through the takeover, and is provided with first valve 14 in the position that is close to the lower extreme of edulcoration cauldron 1 on the takeover, is used for controlling the flow and the velocity of flow of mother liquor after the edulcoration in the edulcoration cauldron 1 to cooling kettle 2. The cooling kettle 2 is arranged at the downstream of the impurity removal kettle 1 and used for cooling and separating out dicyandiamide in the mother liquor after impurity removal, the cooling kettle 2 is connected with the filter 3 through a connecting pipe, and a second valve 24 is arranged on the connecting pipe and close to the lower end of the cooling kettle 2 and used for controlling the flow and the flow velocity of the mother liquor after dicyandiamide crystals are separated out in the cooling kettle and flowing into the filter 3. The filter 3 is arranged at the downstream of the cooling kettle 2 and is used for filtering out dicyandiamide crystals in the mother liquor for separating out dicyandiamide crystals, so that the dicyandiamide crystals are separated from the mother liquor, a mother liquor recovery port 34 is arranged at the lower end of the filter 3 and is used for recovering the mother liquor, and a third valve 35 is further arranged at the position of the mother liquor recovery port and is used for controlling the collection speed and the collection amount of the mother liquor.
Specifically, as shown in fig. 1, a plurality of impurity removing kettles 1 are provided, the impurity removing kettles 1 are respectively connected with a cooling kettle 2, a condenser 4 is further arranged at the upper end of each impurity removing kettle 1, the condenser 4 is vertically arranged on the impurity removing kettle 1, the condenser 4 is a water condenser, the bottom end of the condenser 4 is connected with the upper end of the impurity removing kettle 1 through a connecting pipe, and a valve is further arranged on the connecting pipe and used for controlling on-off. Be equipped with water inlet 42 on the outer wall of condenser 4, the top is equipped with delivery port 41, and in practical application, lets in the comdenstion water in to water inlet 42, the comdenstion water is equipped with delivery port 41 from locating the top and flows out after 4 inner circulations of condenser, carries out the condensation to the ammonia in 4 chambers of condenser and discharges after transforming into the aqueous ammonia, consequently still is provided with liquid ammonia collection mouth 44 in the bottom of this condenser 4 for collect liquid ammonia. The mother liquid after separating the liquid ammonia can further flow into the impurity removing kettle 1 for removing impurities.
Furthermore, the condenser 4 is made of glass and stainless steel, and a safety valve 43 is further disposed on the upper portion of the condenser 4 for ensuring pressure balance in the condenser 4.
Further, the number of the impurity removing kettles 1 is 2, and the lower ends of the two impurity removing kettles 1 are connected with the cooling kettle 2 through connecting pipes. The impurity removing kettle 1 is a cylindrical closed container, the inner wall of the impurity removing kettle 1 is made of enamel or stainless steel, a stirring motor 51 is arranged at the top end of the impurity removing kettle 1, and a stirring paddle 53 connected with the stirring motor 51 through a stirring rod 52 is arranged inside the impurity removing kettle 1.
Further, the paddle 53 includes two layers of blades, an upper layer of blades and a lower layer of blades. The upper layer of the blades are provided with three blades, the upward inclination angle of each blade is 30-35 degrees, the lower layer of the blades are provided with three blades, and each blade is inclined upwards by 30-35 degrees. The purpose of so setting up the paddle is, does benefit to upper strata reaction liquid and flows downwards, does benefit to lower floor's reaction liquid upflow simultaneously to do benefit to the reaction liquid and mix more easily. And the stirring paddle 53 is driven by the stirring motor 51 to rotate clockwise when viewed from the top.
Preferably, the blade of the upper blade is inclined upward at an angle of 30 °, and the blade of the lower blade is inclined upward at an angle of 30 °.
Further, a mother liquor inlet 15 is arranged at the upper end of the impurity removing kettle 1 and used for adding mother liquor into the impurity removing kettle 1.
Further, in order to accelerate the reaction rate, a catalyst inlet 13 is further arranged on the outer wall of the impurity removing kettle 1 and used for adding a catalyst into the impurity removing kettle 1.
Furthermore, in order to ensure the temperature required by the reaction, a heating jacket 11 is additionally arranged on the outer wall of the impurity removing kettle 1, the heating jacket 11 can carry out temperature control such as heating and cooling on the impurity removing kettle 1 at any time, and the medium in the heating jacket 11 can be steam or hot oil.
Further, in order to control the reaction temperature all the time at an optimal reaction temperature, a temperature monitor 12 is further arranged on the outer wall of the impurity removing kettle 1 and used for monitoring the temperature of the reaction kettle 1 all the time, so that an operator can adjust the temperature in time, and the materials in the impurity removing kettle 1 are controlled.
Further, as shown in fig. 1, the cooling tank 2 is a cylindrical closed container, the inner wall of the cooling tank is made of enamel or stainless steel, a stirring motor 51 is provided at the top end of the cooling tank 2, and a stirring paddle 53 connected to the stirring motor 51 through a stirring rod 52 is provided inside the cooling tank 2. The stirring paddle 53 comprises an upper layer paddle and a lower layer paddle, the upper layer paddle is provided with three blades, the upward inclination angle of each blade is 30-40 degrees, the lower layer paddle is provided with three blades, and each blade is inclined upwards by 30-40 degrees.
Preferably, the blade of the upper blade is inclined upward at an angle of 30 °, and the blade of the lower blade is inclined upward at an angle of 30 °.
Further, a cooling jacket is arranged on the outer wall of the cooling kettle 2, the cooling jacket comprises a cooling inlet 22 arranged at the lower end of the outer wall of the cooling kettle 2 and used for introducing cooling media such as cooling water, and a cooling outlet 23 arranged at the upper end of the outer wall of the cooling kettle 2 and used for discharging the cooling media such as cooling water.
In order to further observe the precipitation condition of dicyandiamide in the reaction liquid in the cooling kettle 2, the upper end of the cooling kettle 2 is provided with a sampling window 21, the reaction liquid in the cooling kettle 2 can be sampled and detected at any time through the sampling window 21, and the dicyandiamide in the reaction liquid can be sufficiently precipitated without waste due to the arrangement.
Furthermore, the filter 3 is designed to be closed, the inner wall of the filter is made of enamel or stainless steel, the filter is located below the level of the cooling kettle 2, a filter tank 31 is arranged in the filter tank 31, filter cloth 32 is filled in the filter tank 31, a compressed air inlet 33 is arranged at the top end of the filter 3 and used for separating dicyandiamide crystallized in the mother liquor through compressed air, and the separated liquid is recovered through a mother liquor recovery port 34 arranged at the lower end of the filter 3.
Preferably, the compressed air inlet 33 is provided with a plurality of compressed air inlets, preferably 2 compressed air inlets.
The working mode is as follows:
it is right to combine practical application below the utility model provides an equipment further explains, as shown in fig. 1, at first carry out the edulcoration with the mother liquor in the glycocyamine production process, the edulcoration mode is for pouring into the mother liquor through the mother liquor entry 15 to edulcoration cauldron 1 into, add the catalyst simultaneously in catalyst entry 13, and start agitator motor 51, it rotates to drive stirring paddle leaf 53, to letting in heating medium in the heating jacket 11, start temperature monitor 12, edulcoration cauldron 1's reaction liquid can produce the ammonia this moment, open the valve between edulcoration cauldron 1 and the condenser 4 this moment, discharge the ammonia after condensing in condenser 4.
Next, the mother liquor after impurity removal is cooled by the cooling kettle 2, dicyandiamide in the mother liquor is separated out, at this time, the stirring motor 51 in the cooling kettle 2 is started, the movable stirring paddle 53 in the cooling kettle 2 rotates, the cooling jacket is started, a cooling medium is introduced into the cooling inlet 22, at this time, the reaction liquid in the cooling kettle 2 can be sampled and detected through the sampling window 21 until the sampling is qualified (dicyandiamide crystals in the reaction liquid are basically and completely separated out), and then the separation of dicyandiamide crystals is completed.
And finally, discharging the mother liquor with the separated dicyandiamide crystals to a filter 3, filtering to remove dicyandiamide, and continuously recycling the mother liquor with the dicyandiamide filtered. In the process of filtering out dicyandiamide, in order to accelerate filtering, compressed air can be introduced into a compressed air inlet 33 arranged at the upper end of the filter 3, so as to improve the filtering efficiency of dicyandiamide. And finally, the mother liquor with dicyandiamide filtered out is recycled and reused through a mother liquor recycling port 34.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention.

Claims (10)

1. The dicyandiamide recovery equipment in the production process of glycocyamine is characterized by comprising an impurity removal kettle, a cooling kettle and a filter, wherein,
the impurity removing kettles are arranged at the upstream of the equipment, the impurity removing kettles comprise a plurality of impurity removing kettles, the impurity removing kettles are respectively connected with the cooling kettle, a condenser is also arranged on each impurity removing kettle, the condenser is vertically arranged on the impurity removing kettles, and the bottom ends of the condensers are connected with the upper ends of the impurity removing kettles through connecting pipes;
the cooling kettles are arranged at the downstream of the impurity removal kettles and are used for cooling and separating out dicyandiamide crystals;
the filter is arranged at the downstream of the cooling kettle and is used for filtering the separated dicyandiamide crystals.
2. The dicyandiamide recycling apparatus in a guanidinoacetic acid production process according to claim 1, wherein the number of the impurity removing kettles is 2, the impurity removing kettles are cylindrical closed containers, a stirring motor is arranged at the top end of each impurity removing kettle, and a stirring paddle connected with the stirring motor through a stirring rod is arranged inside each impurity removing kettle.
3. The dicyandiamide recycling apparatus in a glycocyamine production process according to claim 2, wherein the stirring paddle comprises an upper paddle and a lower paddle, the upper paddle is provided with three blades, each blade is inclined upwards by an angle of 30-35 °, and the lower paddle is provided with three blades, each blade is inclined upwards by an angle of 30-35 °.
4. The dicyandiamide recycling apparatus in a guanidinoacetic acid production process according to claim 2, characterized in that a heating jacket is arranged on the outer wall of the impurity removing kettle, a mother liquor inlet for injecting mother liquor is arranged at the top end of the impurity removing kettle, and a catalyst inlet and a temperature monitor are arranged on the side wall of the impurity removing kettle.
5. The dicyandiamide recycling apparatus in a guanidinoacetic acid production process according to claim 1, wherein the cooling kettle is a cylindrical closed container, a stirring motor is arranged at the top end of the cooling kettle, and a stirring paddle connected with the stirring motor through a stirring rod is arranged inside the cooling kettle.
6. The dicyandiamide recycling apparatus in a guanidinoacetic acid production process according to claim 5, characterized in that said stirring paddle comprises an upper paddle and a lower paddle, three blades are arranged on said upper paddle, and each blade is inclined upwards by an angle of 30-40 °, and three blades are arranged on said lower paddle, and each blade is inclined upwards by an angle of 30-40 °.
7. The dicyandiamide recovery apparatus in a guanidinoacetic acid production process according to claim 5, wherein a cooling jacket is arranged on the outer wall of the cooling kettle, a sampling window is arranged at the top end of the cooling kettle, a cooling inlet is arranged at the bottom end of the side wall of the cooling kettle, and a cooling outlet is arranged at the top end of the side wall of the cooling kettle.
8. The dicyandiamide recycling apparatus in a guanidinoacetic acid production process according to claim 1, characterized in that the filter is designed in a closed manner, a filter tank is arranged in the filter, and filter cloth is padded in the filter tank for filtering dicyandiamide crystals.
9. The dicyandiamide recovery apparatus in a guanidinoacetic acid production process according to claim 8, wherein a compressed air inlet is provided at the top end of said filter for passing compressed air therethrough.
10. The dicyandiamide recovery apparatus in a glycocyamine production process according to claim 9, wherein said compressed air inlet is provided in plurality.
CN201921881600.8U 2019-11-04 2019-11-04 Dicyandiamide recovery plant in glycocyamine production process Active CN211099033U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113578220A (en) * 2021-09-03 2021-11-02 西安博典环保科技有限公司 Device and process for filtering dicyandiamide by surface filter with automatic backwashing function
WO2022048913A1 (en) 2020-09-01 2022-03-10 Evonik Operations Gmbh Method for preparing guanidino acetic acid

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022048913A1 (en) 2020-09-01 2022-03-10 Evonik Operations Gmbh Method for preparing guanidino acetic acid
CN113578220A (en) * 2021-09-03 2021-11-02 西安博典环保科技有限公司 Device and process for filtering dicyandiamide by surface filter with automatic backwashing function

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