CN114632484B - Co-production system and co-production process for refined cysteamine hydrochloride and cysteamine - Google Patents

Co-production system and co-production process for refined cysteamine hydrochloride and cysteamine Download PDF

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CN114632484B
CN114632484B CN202210253623.4A CN202210253623A CN114632484B CN 114632484 B CN114632484 B CN 114632484B CN 202210253623 A CN202210253623 A CN 202210253623A CN 114632484 B CN114632484 B CN 114632484B
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pipeline
cysteamine
jacket
ethanol
distillation
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CN114632484A (en
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徐林冬
丁喊亮
邓伟
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Anhui Shindo Chemical Co ltd
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Anhui Shindo Chemical Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/085—Funnel filters; Holders therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B01D36/003—Filters in combination with devices for the removal of liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B01D36/02—Combinations of filters of different kinds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
    • C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
    • C07C319/12—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by reactions not involving the formation of mercapto groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
    • C07C319/26—Separation; Purification; Stabilisation; Use of additives
    • C07C319/28—Separation; Purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00004—Scale aspects
    • B01J2219/00006—Large-scale industrial plants

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a co-production system of refined cysteamine hydrochloride and cysteamine, which comprises a reaction kettle, a centrifugal machine and a refining tower, wherein a conveying pipeline is communicated between the reaction kettle and the centrifugal machine, a first conveying pump is arranged on a pipeline of the conveying pipeline, a first jacket is arranged on the circumferential outer wall of the reaction kettle, a second jacket is arranged on the circumferential outer wall of the centrifugal machine, and the top of the centrifugal machine is connected with an ethanol distillation kettle through a pipeline; the top of the ethanol distillation kettle is communicated with an ethanol recovery pipeline which is respectively communicated with a first jacket and a second jacket; the bottom of the centrifugal machine is connected with a feed inlet of the refining tower through a feed pipeline, a double-cone oven is arranged on a pipeline of the feed pipeline, and an outlet of the refining tower is connected with a suction filtration device. The invention overcomes the defects of the prior art, has reasonable design, avoids the accumulation phenomenon of materials during suction filtration and drying, improves the product quality, and has higher social use value and application prospect.

Description

Co-production system and co-production process for refined cysteamine hydrochloride and cysteamine
Technical Field
The invention relates to the technical field of cysteamine, in particular to a co-production system and a co-production process of refined cysteamine hydrochloride and cysteamine.
Background
As the level of living of people increases, consumer concerns about the health and safety of animal products increase. The feed is a material basis of animal husbandry, is taken as ration of livestock and aquatic animals, and the sanitation and safety of the feed directly determine the sanitation and safety of animal products to a great extent, thereby affecting the health of wide consumers. The feed additive as the core part of the feed plays an incomparable role in improving the economic benefits of animal husbandry and aquaculture. However, in recent years, with the intensive research of animal nutrition science and the dissolution of related science such as modern molecular biology technology, information network technology and nanotechnology, the use of antibiotics as veterinary drugs and feed additives has raised a series of environmental and social problems. Therefore, how to regulate the growth of livestock and poultry through the neuroendocrine way and how to develop pollution-free and residue-free green feed additives become the problems to be solved by the hot spot of many scholars and livestock operators in the present day. The cystamine hydrochloride, a new green feed additive, can produce depletion effect on somatostatin, thus indirectly affecting the level of growth hormone and hormone related to the growth hormone, and has the functions of promoting animal growth and improving growth performance.
Cysteamine hydrochloride has the advantages of remarkable effect, no species specificity, wide application range, low cost and the like, and still has the problems to be solved in actual operation and scientific research. The synthesis and characterization of cysteamine hydrochloride are all along the previous process by integrating relevant documents at home and abroad, and the technology is not greatly improved and innovated in both technical and other aspects, so that the technology is not greatly developed, and therefore, the technology does not show greater economic benefit. Therefore, extensive research and study of cysteamine hydrochloride is necessary.
Cysteamine (CS) HSCHHzCHzNHz, also called R-Cysteamine, white crystalline powder with melting point of 99-100 ℃ and slightly odor, is easy to dissolve in water and alcohol and is alkaline. Is deliquescent, and the aqueous solution thereof turns dark when contacted with metal ions, and sometimes precipitates, so that the aqueous solution can be used for volumetric analysis titration, nickel, copper, zinc and mercury. It is equivalent to the shuttle-removing product of cysteine, is a component of ethyl phthalide coenzyme A and can be condensed with a plurality of organic matters. The active colored base and amino group contained in the composition have various biological functions, are bioactive substances in animal bodies, and have important physiological effects. Cysteamine has a coloured group in the molecule, which is easily oxidized to disulfide in air, and its hydrochloride is usually used as its substitute.
In the prior art, in order to obtain high-content cysteamine hydrochloride with the content of 98% or more, the cysteamine hydrochloride with the content of 93-95% needs to be recrystallized and refined by ethanol and dried to obtain the cysteamine hydrochloride. Specifically, the preparation method of the high-content cysteamine hydrochloride generally adopts a two-step method, and firstly, the cysteamine hydrochloride crude product with the content of about 93-95% is prepared or purchased commercially; and secondly, recrystallizing the crude product in the first step by ethanol (or ethanol water solution) to obtain refined cysteamine hydrochloride with high content (content of 98% or more).
However, in the above-described preparation method for producing high-content cysteamine hydrochloride by the two-step method, there are the following problems: the material is easy to generate oxidation reaction when contacting with air, meanwhile, the material is easy to be piled up when being filtered and dried, the material does not fully participate in the mass transfer process, the operation time for purifying the material is long (as long as more than 20 days), the steam consumption is large, and the relative labor intensity of workers is high.
Accordingly, the inventor has the problem of providing a co-production system and a co-production process for refining cysteamine hydrochloride and cysteamine, which are expected to achieve the purpose of having more practical value, by keeping the experience of the design development and actual production in the related industry for many years and researching and improving the existing structure and the defects.
Disclosure of Invention
In order to solve the problems mentioned in the background art, the invention provides a co-production system and a co-production process of refined cysteamine hydrochloride and cysteamine.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the co-production system for the refined cysteamine hydrochloride and the cysteamine comprises a reaction kettle, a centrifugal machine and a refining tower, wherein a conveying pipeline is communicated between the reaction kettle and the centrifugal machine, a first conveying pump is arranged on a pipeline of the conveying pipeline, a first jacket is arranged on the circumferential outer wall of the reaction kettle, a second jacket is arranged on the circumferential outer wall of the centrifugal machine, and the top of the centrifugal machine is connected with an ethanol distillation kettle through a pipeline;
the top of the ethanol distillation kettle is communicated with an ethanol recovery pipeline which is respectively communicated with a first jacket and a second jacket;
the bottom of the centrifugal machine is connected with a feed inlet of the refining tower through a feed pipeline, a double-cone oven is arranged on a pipeline of the feed pipeline, and an outlet of the refining tower is connected with a suction filtration device.
Preferably, the suction filtration equipment comprises a shell and a conical mixing cavity, wherein the bottom of the conical mixing cavity is communicated with a two-in-one channel, and one side of the two-in-one channel is communicated with a vacuum suction pump through a suction filtration pipe; the other side of the two-in-one channel is communicated with a dryer through a drying pipeline.
Preferably, a filter cover and a filter element are arranged in the conical mixing cavity, the filter cover is positioned at the upper end of the filter element, the filter cover is of an upward protruding cambered surface structure, and the filter element is of a conical structure;
the filter element comprises activated carbon, a filter screen and PP cotton, and the activated carbon, the filter screen and the PP cotton are sequentially combined from top to bottom.
Preferably, a first rotating shaft is vertically arranged at the bottom of the filter element, and a first motor is arranged at the downward extending end of the first rotating shaft penetrating through the two-in-one channel.
Preferably, the top of the suction filtration equipment is vertically inserted with a rotating main shaft, and the top of the rotating main shaft is provided with a fixed plate;
the outer wall of the rotating main shaft is sleeved with a first driving wheel, the first driving wheel is connected with a second driving wheel through a driving belt in a driving way, the inner wall of the second driving wheel is vertically inserted with a second rotating shaft, and the bottom of the second rotating shaft is provided with a second motor.
Preferably, the upper end of the fixed plate is provided with a cylinder, the output end of the cylinder is connected with a piston rod, the piston rod penetrates through the downward extending end of the rotating main shaft to be provided with a connecting part, and the axial side wall of the connecting part is provided with an arc scraping plate in a surrounding mode.
Preferably, a positioning groove is formed in the bottom of the connecting component, and a positioning lug corresponding to the positioning groove is arranged at the upper end of the filter cover.
A co-production process of refined cysteamine hydrochloride and cysteamine comprises the following steps:
s1: pumping ethanol into the reaction kettle by a metering pump, weighing a cysteamine hydrochloride crude product between closed feeding, filling the cysteamine hydrochloride crude product into a closed ton bag, opening a manhole cover, adding the cysteamine hydrochloride crude product under the condition of micro negative pressure of the reaction kettle by travelling crane, and starting stirring;
s2: opening a steam valve, controlling the steam pressure to be not more than 0.2MPa, heating to 70 ℃ after 1.5h, stirring for 0.5h, dissolving, opening first jacket cooling water for cooling, and cooling to 20 ℃ after 3 h;
s3: pumping materials in the reaction kettle into a centrifuge through a conveying pipeline to start centrifugation, and putting the obtained solid into a biconical oven through the conveying pipeline to dry to obtain a cysteamine hydrochloride finished product;
s4: transferring the crystallized ethanol mother liquor in the centrifuge in the S3 to an ethanol distillation kettle, maintaining the temperature at 80 ℃ and recovering ethanol at normal pressure to obtain ethanol steam for jacket heating, and treating distillation residual liquid as waste liquid;
s5: pumping the cysteamine hydrochloride finished product in the step S3 into a refining tower, and adding water through a water flow meter; weighing sodium hydroxide between closed feeding, adding in 5 batches, performing neutralization reaction, controlling the temperature to be 10-50 ℃, starting distillation after 2 hours of neutralization, controlling the steam pressure to be 0.3MPa, controlling the temperature to be 110 ℃, and performing vacuum to be 0.09MPa for 5 hours, wherein after one-time distillation, the cysteamine aqueous solution is obtained, and the distillation residues are used as solid waste for treatment;
s6: performing secondary distillation on the cysteamine aqueous solution in the step S5, controlling the temperature to 90 ℃, performing vacuum-0.09 MPa for 10 hours, after the secondary distillation is finished, pumping methanol into a refining kettle by a metering pump, starting steam, controlling the steam pressure to be within 0.1MPa, heating to 65 ℃ for dissolution, cooling jacket brine to 0-10 ℃, performing filtration by a suction filtration device, performing drying, controlling the temperature to 30-40 ℃, performing vacuum-0.09 MPa for 5 hours, and packaging to obtain a cysteamine finished product;
the water recovered by the secondary distillation is directly reused for neutralization and feeding; transferring the crystallized methanol mother liquor to a methanol distillation kettle, recovering the crystallized methanol at the temperature of 70 ℃ and under normal pressure to obtain recovered methanol for recrystallization, and treating distillation residues as solid waste.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the ethanol is recovered by arranging the ethanol distillation kettle, and is introduced into the jacket for heating, so that the energy is saved, and the economic benefit is improved;
in the invention, the cysteamine is refined through primary distillation and secondary distillation, so that the purity of the cysteamine is improved;
according to the invention, the rotation of the filter cover and the rotation of the arc-shaped scraping plate in the suction filtration equipment are utilized to scrape off the finished product materials, so that the finished product materials are sufficiently dispersed, the materials are enhanced to sufficiently participate in the mass transfer process, and the quality of the finished product is improved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of a process flow of the present invention;
FIG. 2 is a schematic diagram of a system flow of the present invention;
FIG. 3 is a schematic diagram of a suction filtration apparatus according to the present invention;
fig. 4 is an enlarged schematic view of the structure a of the present invention.
In the figure: the device comprises a reaction kettle 1, a centrifugal machine 2, an ethanol distillation kettle 3, a refining tower 4, a suction filtration device 5, a filter cover 51, a filter element 52, active carbon 521, a filter screen 522, PP cotton 523, a two-in-one channel 53, a suction filtration pipe 54, a vacuum pump 55, a drying pipeline 56, a dryer 57, a first motor 58, a rotating main shaft 59, a piston rod 510, a connecting part 511, an arc scraping plate 512, a positioning groove 513, a fixed plate 514, a cylinder 515, a first driving wheel 516, a driving belt 517, a second driving wheel 518, a second motor 519, a discharge hole 520, a biconical oven 6, a first jacket 7, a second jacket 8, a conveying pipeline 9, a first conveying pump 10, a booster pump 11, a second conveying pump 12, an ethanol recovery pipeline 13, a feeding pipeline 14 and a reboiler 15.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1-4, a co-production system of refined cysteamine hydrochloride and cysteamine comprises a reaction kettle 1, a centrifugal machine 2 and a refining tower 4, wherein a conveying pipeline 9 is communicated between the reaction kettle 1 and the centrifugal machine 2, a first conveying pump 10 is arranged on a pipeline of the conveying pipeline 9, a first jacket 7 is arranged on the circumferential outer wall of the reaction kettle 1, a second jacket 8 is arranged on the circumferential outer wall of the centrifugal machine 2, and the top of the centrifugal machine 2 is connected with an ethanol distillation kettle 3 through a pipeline;
the top of the ethanol distillation kettle 3 is communicated with an ethanol recovery pipeline 13, and the ethanol recovery pipeline 13 is respectively communicated with a first jacket 7 and a second jacket 8; the first jacket 7 and the second jacket 8 are filled with cooling water for cooling treatment, ethanol gas is filled for heating, and the recovered ethanol heat is utilized for heating, so that energy sources are saved, and economic benefits are improved;
the bottom of the centrifugal machine 2 is connected with the feed inlet of the refining tower 4 through a feed pipeline 14, a biconical oven 6 is arranged on the pipeline of the feed pipeline 14, the outlet of the refining tower 4 is connected with a suction filtration device 5, the bottom of the refining tower 4 is connected with a reboiler 15, a second delivery pump 12 is arranged on the pipeline of the feed pipeline 14,
the suction filtration equipment 5 comprises a shell and a conical mixing cavity, wherein the bottom of the conical mixing cavity is communicated with a two-in-one channel 53, and one side of the two-in-one channel 53 is communicated with a vacuum suction pump 55 through a suction filtration pipe 54; the other side of the two-in-one channel 53 is communicated with a dryer 57 through a drying pipeline 56.
The filter cover 51 and the filter element 52 are arranged in the conical mixing cavity, the filter cover 51 is positioned at the upper end of the filter element 52, the filter element 52 comprises active carbon 521, a filter screen 522 and PP cotton 523, the active carbon 521, the filter screen 522 and the PP cotton 523 are sequentially combined from top to bottom, the filter cover 51 is of an upward protruding cambered surface structure, a finished product is convenient to gather towards the bottom, and accordingly output is convenient to achieve, the filter element 52 is of a conical structure, and suction filtration and drying are convenient after the vacuum suction pump 55 is started;
the bottom of the filter element 52 is vertically provided with a first rotating shaft, a first motor 58 is arranged at the downward extending end of the first rotating shaft penetrating through the two-in-one channel 53, and the first motor 58 is started to drive the filter element 52 and the filter cover 51 to rotate, so that materials are fully dispersed, and subsequent suction filtration and drying are facilitated; valves are respectively arranged on the pipelines of the suction filtration pipe 54 and the drying pipeline 56; when the vacuum pump 55 is started, the valve on the drying pipeline 56 is closed; when dryer 57 is started, the valve on the line of suction filter tube 54 is closed;
a rotating main shaft 59 is vertically inserted at the top of the suction filtration equipment 5, and a fixed plate 514 is arranged at the top of the rotating main shaft 59; the outer wall of the rotary main shaft 59 is sleeved with a first driving wheel 516, the first driving wheel 516 is connected with a second driving wheel 518 through a driving belt 517 in a driving way, the inner wall of the second driving wheel 518 is vertically inserted with a second rotating shaft, and the bottom of the second rotating shaft is provided with a second motor 519.
The upper end of the fixed plate 514 is provided with a cylinder 515, the output end of the cylinder 515 is connected with a piston rod 510, the downward extending end of the piston rod 510 penetrating through the rotating main shaft 59 is provided with a connecting part 511, and the axial side wall of the connecting part 511 is provided with an arc scraping plate 512 in a surrounding manner.
The bottom of the connecting component 511 is provided with a positioning groove 513, the upper end of the filter cover 51 is provided with a positioning lug corresponding to the positioning groove 513, when the filter cover is used, the cylinder 515 is started, the piston rod 510 is driven to extend downwards, the connecting component 511 and the arc-shaped scraping plate 512 are driven to move downwards until the positioning groove 513 abuts against the positioning lug, the piston rod 510 is stopped from being driven downwards, and then the second motor 519 is started;
the second motor 519 drives the second driving wheel 518 to rotate through the second rotating shaft, the second driving wheel 518 drives the first driving wheel 516 to rotate through the driving belt 517, the first driving wheel 516 drives the rotating main shaft 59 to rotate, the rotating main shaft 59 drives the arc scraping plate 512 to rotate, scraping of materials is achieved, the drying effect is prevented from being influenced by material accumulation, meanwhile, under the autorotation effect of the filter cover 51, the materials are further enhanced to fully participate in the mass transfer process, and the discharging port 520 is opened to be output outwards after a final product.
A co-production process of refined cysteamine hydrochloride and cysteamine comprises the following steps:
s1: pumping ethanol into the reaction kettle 1 by a metering pump, weighing a cysteamine hydrochloride crude product between closed feeding, filling the cysteamine hydrochloride crude product into a closed ton bag, opening a manhole cover, adding the cysteamine hydrochloride crude product under the condition of micro negative pressure of the reaction kettle by travelling crane, and starting stirring;
s2: opening a steam valve, controlling the steam pressure to be not more than 0.2MPa, heating to 70 ℃ after 1.5h, stirring for 0.5h, dissolving, opening a first jacket 7, cooling with cooling water, and cooling to 20 ℃ after 3 h;
s3: pumping materials in the reaction kettle 1 into a centrifugal machine 2 through a conveying pipeline 9 to start centrifugation, and putting the obtained solid into a biconical oven 6 through a conveying pipeline 14 to dry to obtain a cysteamine hydrochloride finished product;
s4: transferring the crystallized ethanol mother liquor in the centrifuge 2 in the S3 to an ethanol distillation kettle 3, maintaining the temperature at 80 ℃ and recovering ethanol at normal pressure to obtain ethanol steam for jacket heating, and treating distillation residual liquid as waste liquid;
s5: pumping the cysteamine hydrochloride finished product in the step S3 into the refining tower 4, and adding water through a water flow meter; weighing sodium hydroxide between closed feeding, adding in 5 batches, performing neutralization reaction, controlling the temperature to be 10-50 ℃, starting distillation after 2 hours of neutralization, controlling the steam pressure to be 0.3MPa, controlling the temperature to be 110 ℃, and performing vacuum to be 0.09MPa for 5 hours, wherein after one-time distillation, the cysteamine aqueous solution is obtained, and the distillation residues are used as solid waste for treatment;
s6: performing secondary distillation on the cysteamine aqueous solution in the step S5, controlling the temperature to 90 ℃, carrying out vacuum-0.09 MPa for 10 hours, after the secondary distillation is finished, pumping methanol into a refining kettle 4 by a metering pump, starting steam, controlling the steam pressure to be within 0.1MPa, heating to 65 ℃ for dissolution, cooling jacket brine to 0-10 ℃, filtering by a suction filtration device 5, drying, controlling the temperature to 30-40 ℃, carrying out vacuum-0.09 MPa for 5 hours, and packaging to obtain a cysteamine finished product;
the water recovered by the secondary distillation is directly reused for neutralization and feeding; transferring the crystallized methanol mother liquor to a methanol distillation kettle, recovering at 70 ℃ under normal pressure to obtain recovered methanol for recrystallization, treating distillation residues by solid waste, and ensuring that cysteamine is easily oxidized, and introducing nitrogen for protection in all processes to ensure that the content is qualified.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; the connection may be mechanical connection, direct connection or indirect connection through an intermediate medium, and may be internal connection of two elements or interaction relationship of two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The control mode of the invention is automatically controlled by the controller, the control circuit of the controller can be realized by simple programming of a person skilled in the art, the supply of power also belongs to common knowledge in the art, and the invention is mainly used for protecting a mechanical device, so the invention does not explain the control mode and circuit connection in detail.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (2)

1. The utility model provides a coproduction system of refined cysteamine hydrochloride and cysteamine, includes reation kettle (1), centrifuge (2) and refining tower (4), the intercommunication has pipeline (9) between reation kettle (1) and centrifuge (2), installs first delivery pump (10), its characterized in that on the pipeline of pipeline (9):
the method comprises the steps that a first jacket (7) is arranged on the circumferential outer wall of a reaction kettle (1), a second jacket (8) is arranged on the circumferential outer wall of a centrifugal machine (2), and the top of the centrifugal machine (2) is connected with an ethanol distillation kettle (3) through a pipeline;
the top of the ethanol distillation kettle (3) is communicated with an ethanol recovery pipeline (13), and the ethanol recovery pipeline (13) is respectively communicated with a first jacket (7) and a second jacket (8);
the bottom of the centrifugal machine (2) is connected with a feed inlet of the refining tower (4) through a feed pipeline (14), a double-cone oven (6) is arranged on a pipeline of the feed pipeline (14), and an outlet of the refining tower (4) is connected with a suction filtration device (5);
the suction filtration equipment (5) comprises a shell and a conical mixing cavity, wherein the bottom of the conical mixing cavity is communicated with a two-in-one channel (53), and one side of the two-in-one channel (53) is communicated with a vacuum suction pump (55) through a suction filtration pipe (54); the other side of the two-in-one channel (53) is communicated with a dryer (57) through a drying pipeline (56); valves are respectively arranged on the pipelines of the suction filtration pipe (54) and the drying pipeline (56); when the vacuum sucking pump (55) is started, a valve on a pipeline of the drying pipeline (56) is closed; when the dryer (57) is started, the valve on the suction filtration tube (54) pipeline is closed;
the conical mixing cavity is internally provided with a filter cover (51) and a filter element (52), the filter cover (51) is positioned at the upper end of the filter element (52), the filter cover (51) is of an upward protruding cambered surface structure, and the filter element (52) is of a conical structure;
the filter element (52) comprises active carbon (521), a filter screen (522) and PP cotton (523), and the active carbon (521), the filter screen (522) and the PP cotton (523) are sequentially combined from top to bottom;
the bottom of the filter element (52) is vertically provided with a first rotating shaft, and a first motor (58) is arranged at the downward extending end of the first rotating shaft penetrating through the two-in-one channel (53);
a rotating main shaft (59) is vertically inserted into the top of the suction filtration equipment (5), and a fixing plate (514) is arranged on the top of the rotating main shaft (59);
the outer wall of the rotating main shaft (59) is sleeved with a first driving wheel (516), the first driving wheel (516) is in driving connection with a second driving wheel (518) through a driving belt (517), a second rotating shaft is vertically inserted into the inner wall of the second driving wheel (518), and a second motor (519) is arranged at the bottom of the second rotating shaft;
the upper end of the fixed plate (514) is provided with an air cylinder (515), the output end of the air cylinder (515) is connected with a piston rod (510), the downward extending end of the piston rod (510) penetrating through the rotating main shaft (59) is provided with a connecting component (511), and the axial side wall of the connecting component (511) is provided with an arc scraping plate (512) in a surrounding mode;
the bottom of the connecting component (511) is provided with a positioning groove (513), and the upper end of the filter cover (51) is provided with a positioning lug corresponding to the positioning groove (513).
2. A co-production process of refined cysteamine hydrochloride and cysteamine, which adopts the co-production system of refined cysteamine hydrochloride and cysteamine according to claim 1, and is characterized by comprising the following steps:
s1: pumping ethanol into a reaction kettle (1) by a metering pump, weighing a cysteamine hydrochloride crude product between closed feeding, filling the cysteamine hydrochloride crude product into a closed ton bag, opening a manhole cover, adding the cysteamine hydrochloride crude product under the condition of micro negative pressure of the reaction kettle by travelling crane, and starting stirring;
s2: opening a steam valve, controlling the steam pressure to be not more than 0.2MPa, heating to 70 ℃ after 1.5h, stirring for 0.5h, dissolving, opening a first jacket (7) for cooling by cooling water, and cooling to 20 ℃ after 3 h;
s3: pumping materials in the reaction kettle (1) into a centrifugal machine (2) through a conveying pipeline (9) to start centrifugation, and putting the obtained solid into a biconical oven (6) through a conveying pipeline (14) to dry to obtain a cysteamine hydrochloride finished product;
s4: transferring the crystallized ethanol mother liquor in the centrifuge (2) in the S3 to an ethanol distillation kettle (3), maintaining the temperature at 80 ℃ and recovering ethanol at normal pressure to obtain ethanol steam for jacket heating, and treating the distillation residual liquor as waste liquor;
s5: pumping the cysteamine hydrochloride finished product in the S3 into a refining tower (4), and adding water through a water flow meter; weighing sodium hydroxide between closed feeding, adding in 5 batches, performing neutralization reaction, controlling the temperature to be 10-50 ℃, starting distillation after 2 hours of neutralization, controlling the steam pressure to be 0.3MPa, controlling the temperature to be 110 ℃, and performing vacuum to be 0.09MPa for 5 hours, wherein after one-time distillation, the cysteamine aqueous solution is obtained, and the distillation residues are used as solid waste for treatment;
s6: and (3) carrying out secondary distillation on the cysteamine aqueous solution in the step (S5), controlling the temperature to 90 ℃, carrying out vacuum-0.09 MPa for 10 hours, after the secondary distillation is finished, pumping methanol into a refining tower (4) by a metering pump, starting steam, controlling the steam pressure to be within 0.1MPa, heating to 65 ℃ for dissolution, cooling jacket brine to 0-10 ℃, filtering by a suction filtration device (5), drying, controlling the temperature to 30-40 ℃, carrying out vacuum-0.09 MPa for 5 hours, and packaging to obtain a cysteamine finished product.
CN202210253623.4A 2022-03-15 2022-03-15 Co-production system and co-production process for refined cysteamine hydrochloride and cysteamine Active CN114632484B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102260202A (en) * 2010-05-25 2011-11-30 陈士安 Method for producing 2-amino-3-mercaptopropionic acid
CN104645690A (en) * 2015-02-11 2015-05-27 合肥通用机械研究院 Layered multi-filter disc filter
CN109503441A (en) * 2017-09-15 2019-03-22 阜新达得利化工股份有限公司 The preparation method of high-content Mercaptamine

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102260202A (en) * 2010-05-25 2011-11-30 陈士安 Method for producing 2-amino-3-mercaptopropionic acid
CN104645690A (en) * 2015-02-11 2015-05-27 合肥通用机械研究院 Layered multi-filter disc filter
CN109503441A (en) * 2017-09-15 2019-03-22 阜新达得利化工股份有限公司 The preparation method of high-content Mercaptamine

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