CN111905674A - Imino disuccinate apparatus for producing - Google Patents

Imino disuccinate apparatus for producing Download PDF

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Publication number
CN111905674A
CN111905674A CN201911385809.XA CN201911385809A CN111905674A CN 111905674 A CN111905674 A CN 111905674A CN 201911385809 A CN201911385809 A CN 201911385809A CN 111905674 A CN111905674 A CN 111905674A
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CN
China
Prior art keywords
reactor
iminodisuccinate
solid
liquid
temperature
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Withdrawn
Application number
CN201911385809.XA
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Chinese (zh)
Inventor
常领山
张杰纯
朱洪波
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Shandong Yuanlian Chemical Co ltd
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Shandong Yuanlian Chemical Co ltd
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Priority to CN201911385809.XA priority Critical patent/CN111905674A/en
Publication of CN111905674A publication Critical patent/CN111905674A/en
Withdrawn legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/002Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/007Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/14Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
    • C07C227/18Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • B01J2219/00063Temperature measurement of the reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00132Controlling the temperature using electric heating or cooling elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00177Controlling or regulating processes controlling the pH
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00182Controlling or regulating processes controlling the level of reactants in the reactor vessel

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention belongs to the technical field of production of iminodisuccinate, and particularly relates to a production device of iminodisuccinate, which comprises a reaction device (1), a temperature adjusting device (2) and a detection device (3). The method has the advantages of mild reaction conditions, low requirement on equipment materials and low manufacturing cost; automatic control is set, so that the labor intensity of personnel operation is reduced, and the error rate is reduced; automatic control is set, and the product quality is stable.

Description

Imino disuccinate apparatus for producing
Technical Field
The invention belongs to the technical field of production of imino disuccinate in fertilizer, and particularly relates to an imino disuccinate production device.
Background
With the richness of the country, agriculture obtains continuous high yield. The yield is stable and increased in agriculture, and fertilizer synergist can not be used. In the fertilizer synergist, the chelating synergist occupies the half-wall Jiangshan.
The chelating synergist is rich in a plurality of active groups (carboxyl, amino, amido and the like), can activate trace elements (potassium, calcium, iron, zinc, magnesium, copper and the like) in soil and fertilizers, promotes the absorption and utilization of plants, and has the effects of reducing weight, increasing yield and enhancing effect.
The iminodisuccinate is a novel aminocarboxylic acid chelating agent, has strong capability of chelating transition metal ions and alkali metal ions, particularly has excellent chelating ability to iron and copper metal ions, and exceeds the chelating ability of EDTA. In addition, compared with the conventional chelating agents such as phosphate, citric acid, EDTA and the like, the iminodisuccinate has remarkably superior biodegradability and is nontoxic and harmless to an ecosystem, so that the iminodisuccinate is regarded as a green chelating agent and has good market acceptance.
At present, the production methods of the iminodisuccinate chelating agent are mainly two methods as follows:
1. the Langsheng company uses maleic anhydride and ammonia as raw materials, adds a proper amount of sodium hydroxide to adjust the pH value of a system, and then completes reaction under the conditions of high temperature and high pressure to obtain a mixed liquid product containing a chelating agent, wherein the content of the chelating agent in the solid of the mixed liquid product is higher than 70%. However, the high-temperature high-pressure reaction brings great potential safety hazard, and has very high requirements on various aspects such as matched equipment type selection, factory building design, space arrangement, production process management and the like, so that the production investment of the iminodisuccinate is high, the energy consumption is high, the cost is high, and the danger is great; in addition, the ammonia raw material can seriously pollute the environment in the using process and harm the personal health of operators.
2. Chinese patent CN1126733C discloses a preparation method of an iminodisuccinate chelating agent. The method takes maleic anhydride and ammonia as raw materials, and greatly improves the reaction yield by controlling the pH value of a reaction system, so that the conversion rate of the maleic anhydride reaches more than 97 percent. However, the method still adopts high-temperature high-pressure reaction, and the problems of potential safety hazard and environmental pollution caused by the high-temperature high-pressure reaction cannot be solved.
Based on this, it is highly desirable to provide an iminodisuccinate production apparatus capable of automatically producing iminodisuccinate under normal pressure conditions.
Disclosure of Invention
The invention provides an imino disuccinate production device, which is used for solving the problems in the prior art.
An imino disuccinate production device comprises a reaction device, a temperature adjusting device and a detection device;
the reaction device comprises a reactor, wherein a solid feeding hole, a liquid feeding hole and a discharging hole are formed in the reactor, the solid feeding hole is formed in the upper portion of the reactor, the liquid feeding hole is formed in the upper portion of the reactor, and the discharging hole is formed in the lower portion of the reactor;
the temperature adjusting device is arranged on the reactor and adopts at least one of a jacket, a coil pipe and an electric heating device, the jacket and the coil pipe exchange heat with materials in the reactor through internal heating media, and the heat exchange comprises heating and/or cooling;
the detection device comprises a thermometer, and the thermometer is arranged on the reactor and used for measuring the temperature inside the reactor.
Further, the reactor used a 316L stainless steel kettle.
Further, the reaction device also comprises a stirrer. The stirrer is arranged on the reactor and used for promoting the materials in the reactor to be uniformly mixed.
Further, the detection device also comprises a pH meter which is arranged on the reactor and used for measuring the pH value inside the reactor.
Further, the reactor adopts at least one of a tubular reactor and a kettle type reactor.
Further, the iminodisuccinate production plant also comprises a liquid feed device, and the liquid feed device comprises a liquid storage tank; and the outlet of the liquid storage tank is connected with the liquid feeding hole.
Further, there is more than one liquid feed device.
Further, detection device still includes the level gauge, the level gauge sets up on the liquid storage tank for measure the inside liquid level of liquid storage tank.
Further, the liquid level meter is connected with the opening degree of the valve at the liquid feed inlet. When the liquid level difference of the liquid level meter reaches a preset value, the valve at the liquid feed inlet is automatically closed.
Further, the iminodisuccinate production device also comprises a solid feeding device, wherein the solid feeding device comprises a solid storage tank and a solid feeder; the inlet of the solid feeder is connected with the outlet of the solid storage tank, and the outlet of the solid feeder is connected with the solid feeding hole.
Further, the bottom of the solid storage tank is conical, and the outlet of the solid storage tank is arranged at the bottommost part of the conical shape.
Further, the solid feeder adopts at least one of a conveyor belt and a screw feeder.
Further, the solid feed device is more than one. Respectively adding a raw material A and a raw material B, wherein the raw material A is selected from maleic anhydride or maleic acid derivatives, and the raw material B is aspartic acid.
Further, the thermometer is connected with the temperature adjusting device switch;
when the temperature adjusting device adopts a jacket and/or a coil, the thermometer is connected with the opening of the outlet and/or inlet valve of the temperature adjusting device, and the temperature is automatically controlled by automatically adjusting the opening of the valve;
when the temperature adjusting device adopts an electric heating device, the temperature measuring device is linked with the heat exchange device through current, and the temperature is automatically controlled through automatically adjusting the current.
Further, the imino disuccinate production device further comprises an alarm, the alarm is connected with the detection device, and when the numerical value of the detection device exceeds a preset value, the alarm gives an alarm. When the liquid level of the liquid level meter exceeds the highest preset value and/or the lowest preset value, the alarm gives an alarm; and when the thermometer exceeds a preset value, the alarm gives an alarm.
Further, the imino disuccinate production device also comprises a filtering device, and the filtering device is connected with the discharge hole. The filtering device is used for filtering solid impurity particles in a product, and the filtrate is the product and can be directly canned for sale.
When the solid caustic soda liquid is used, water is added into the liquid storage tank, the raw material A, the raw material B and the flake caustic soda are respectively added into the solid storage tank, and the addition amount of the water, the addition amount of the raw material A and the addition amount of the raw material B are preset. Under the control of an automatic control system, the automatic operation is carried out according to the following steps:
quantitatively adding water into the reactor from the liquid storage tank;
quantitatively adding the raw material B into the reactor by the solid feeding device, and uniformly stirring;
quantitatively adding the raw material A into the reactor by the solid feeding device, and uniformly stirring;
under the conditions of stirring and controlling the temperature to be 70 ℃, the solid feeding device quantitatively adds flake caustic soda (the flake caustic soda can also be configured into a solution which is quantitatively dripped into the reactor from the liquid storage tank), the change rate of the pH value measured by the pH meter controls the valve opening of the liquid feed inlet, so that the addition rate of the alkali liquor is controlled, the reaction is ensured to be uniformly carried out, and the local alkali liquor concentration in the reactor is prevented from being too high;
adding alkali, heating to 90-100 deg.C, maintaining for 24 hr, and testing, if qualified, ending production; if not, cooling to 70 ℃, adding alkali for the second time, and then heating for reaction.
The temperature value measured by the thermometer controls the opening of the temperature adjusting device, so that the temperature is relatively constant (the reaction temperature is controlled within the range of 70-120 ℃).
The invention has the beneficial effects that:
1. the reaction condition is mild, the requirement on equipment material is low, and the manufacturing cost is low;
2. automatic control is set, so that the labor intensity of personnel operation is reduced, and the error rate is reduced;
3. automatic control is set, and the product quality is stable.
Drawings
FIG. 1 is a schematic view of a connection structure according to the present invention;
FIG. 2 is a schematic view of a reaction apparatus according to the present invention;
FIG. 3 is a schematic view of the structure of the solid feeding device of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are only some embodiments, but not all embodiments, of the present invention. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without any creative effort, belong to the protection scope of the present invention.
Example 1
An imino disuccinate production device comprises a reaction device 1, a temperature adjusting device 2 and a detection device 3;
the reaction device 1 comprises a reactor 11 and a stirrer 12, wherein a solid feeding hole 111, a liquid feeding hole 112 and a discharging hole 113 are formed in the reactor 11, the solid feeding hole 111 is formed in the upper portion of the reactor 11, the liquid feeding hole 112 is formed in the upper portion of the reactor 11, and the discharging hole 113 is formed in the lower portion of the reactor 11; the stirrer 12 is arranged on the reactor 11 and used for promoting the materials in the reactor 11 to be uniformly mixed;
the temperature adjusting device 2 is arranged on the reactor 11, the temperature adjusting device 2 adopts at least one of a jacket, a coil and an electric heating device, the jacket and the coil exchange heat with materials in the reactor 11 through internal heating media, and the heat exchange comprises heating and/or cooling;
the detecting means 3 includes a thermometer 31, and the thermometer 31 is provided on the reactor 11 for measuring the internal temperature of the reactor 11.
In the embodiment, the thermometer 31 is connected with the temperature adjusting device 2 through a switch;
when the temperature adjusting device 2 adopts a jacket and/or a coil, the thermometer 31 is connected with the opening of an outlet and/or inlet valve of the temperature adjusting device 2, and the temperature is automatically controlled by automatically adjusting the opening of the valve;
when the temperature adjusting device 2 adopts an electric heating device, the temperature measuring device is connected with the heat exchange device through current, and the temperature is automatically controlled by automatically adjusting the current.
In this embodiment, the iminodisuccinate production apparatus further comprises a liquid feeding device 4, wherein the liquid feeding device 4 comprises a liquid storage tank 41; the outlet of the liquid storage tank 41 is connected with the liquid feed port 112.
In this embodiment, the detecting device 3 further includes a liquid level meter 33, and the liquid level meter 33 is disposed on the liquid storage tank 41 and is used for measuring the liquid level inside the liquid storage tank 41.
In the embodiment, the liquid level meter 33 is connected with the opening degree of the valve at the liquid inlet 112.
In the embodiment, the solid feeding device 5 is further included, and the solid feeding device 5 includes a solid storage tank 51, a solid feeder 52; the inlet of the solid feeder 52 is connected with the outlet of the solid storage tank 51, and the outlet of the solid feeder 52 is connected with the solid feeding hole 111.
In the embodiment, the solid feeder 52 is at least one of a conveyor belt and a screw feeder.
In this embodiment, the device further includes a filtering device 7, and the filtering device 7 is connected to the discharge port 113.
In this embodiment, the detecting device 3 further includes a pH meter 32, and the pH meter 32 is disposed on the reactor 11 for measuring the pH value inside the reactor 11.
In this embodiment, still include alarm 6, alarm 6 with detection device 3 links to each other and locks, when detection device 3's numerical value exceeded the default, alarm 6 takes place to report to the police.
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; while the invention has been described in detail and with reference to the foregoing embodiments, it will 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; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The device for producing the iminodisuccinate is characterized by comprising a reaction device (1), a temperature adjusting device (2) and a detection device (3);
the reaction device (1) comprises a reactor (11) and a stirrer (12), wherein a solid feeding hole (111), a liquid feeding hole (112) and a discharging hole (113) are formed in the reactor (11), the solid feeding hole (111) is formed in the upper portion of the reactor (11), the liquid feeding hole (112) is formed in the upper portion of the reactor (11), and the discharging hole (113) is formed in the lower portion of the reactor (11); the stirrer (12) is arranged on the reactor (11) and used for promoting the materials in the reactor (11) to be uniformly mixed;
the temperature adjusting device (2) is arranged on the reactor (11), the temperature adjusting device (2) adopts at least one of a jacket, a coil and an electric heating device, the jacket and the coil exchange heat with materials in the reactor (11) through an internal heating medium, and the heat exchange comprises heating and/or cooling;
the detection device (3) comprises a thermometer (31), and the thermometer (31) is arranged on the reactor (11) and used for measuring the internal temperature of the reactor (11).
2. Iminodisuccinate production device according to claim 1, wherein said thermometer (31) is in on-off interlock with said temperature regulating device (2);
when the temperature adjusting device (2) adopts a jacket and/or a coil, the thermometer (31) is connected and locked with the opening of the outlet and/or inlet valve of the temperature adjusting device (2), and the temperature is automatically controlled by automatically adjusting the opening of the valve;
when the temperature adjusting device (2) adopts an electric heating device, the temperature measuring device is connected with the heat exchange device in a current locking way, and the temperature is automatically controlled by automatically adjusting the current.
3. An iminodisuccinate production plant according to claim 1, further comprising a liquid feed means (4), said liquid feed means (4) comprising a liquid storage tank (41); the outlet of the liquid storage tank (41) is connected with the liquid feeding hole (112).
4. Iminodisuccinate production device according to claim 3, wherein said detection device (3) further comprises a level gauge (33), said level gauge (33) being arranged on said liquid tank (41) for measuring the liquid level inside said liquid tank (41).
5. An iminodisuccinate production plant according to claim 4, wherein said level gauge (33) is interlocked with the valve opening at the liquid feed inlet (112).
6. An iminodisuccinate production plant according to claim 1, further comprising a solid feeding device (5), said solid feeding device (5) comprising a solid storage tank (51), a solid feeder (52); the inlet of the solid feeder (52) is connected with the outlet of the solid storage tank (51), and the outlet of the solid feeder (52) is connected with the solid feeding hole (111).
7. An iminodisuccinate production plant according to claim 6, wherein said solids feeder (52) is at least one of a conveyor belt, a screw feeder.
8. An iminodisuccinate production device according to claim 1, further comprising a filtration device (7), wherein said filtration device (7) is connected to said outlet port (113).
9. Iminodisuccinate production device according to claim 1, characterized in that said detection device (3) further comprises a pH meter (32), said pH meter (32) being arranged on said reactor (11) for measuring the pH value inside said reactor (11).
10. An iminodisuccinate production device according to any of claims 1-9, further comprising an alarm (6), wherein said alarm (6) is connected to said detection device (3), and wherein said alarm (6) is configured to alarm when the value of said detection device (3) exceeds a predetermined value.
CN201911385809.XA 2019-12-29 2019-12-29 Imino disuccinate apparatus for producing Withdrawn CN111905674A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111620790A (en) * 2019-12-31 2020-09-04 曹清清 Production method and production device of glycine diacetic acid derivative chelating agent
CN111892515A (en) * 2019-12-29 2020-11-06 山东远联化工股份有限公司 Production method and production device of carbamido chelating agent

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111892515A (en) * 2019-12-29 2020-11-06 山东远联化工股份有限公司 Production method and production device of carbamido chelating agent
CN111620790A (en) * 2019-12-31 2020-09-04 曹清清 Production method and production device of glycine diacetic acid derivative chelating agent

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Application publication date: 20201110