CN115582082B - System and process for producing aluminum hydroxide adjuvant based on-line detection and control system - Google Patents

System and process for producing aluminum hydroxide adjuvant based on-line detection and control system Download PDF

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CN115582082B
CN115582082B CN202211272535.5A CN202211272535A CN115582082B CN 115582082 B CN115582082 B CN 115582082B CN 202211272535 A CN202211272535 A CN 202211272535A CN 115582082 B CN115582082 B CN 115582082B
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online detection
detection system
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aluminum chloride
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CN115582082A (en
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杜翔宇
李景良
李宗原
王选迎
裴友亮
刘智慧
韩慧利
翟东颖
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Changchun Institute of Biological Products
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    • 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
    • B01J19/0053Details of the reactor
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K39/00Medicinal preparations containing antigens or antibodies
    • A61K39/39Medicinal preparations containing antigens or antibodies characterised by the immunostimulating additives, e.g. chemical adjuvants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/003Filters in combination with devices for the removal of liquids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20Measuring; Control or regulation
    • B01F35/21Measuring
    • B01F35/211Measuring of the operational parameters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20Measuring; Control or regulation
    • B01F35/21Measuring
    • B01F35/2132Concentration, pH, pOH, p(ION) or oxygen-demand
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71Feed mechanisms
    • B01F35/717Feed mechanisms characterised by the means for feeding the components to the mixer
    • B01F35/7176Feed mechanisms characterised by the means for feeding the components to the mixer using pumps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B5/00Other centrifuges
    • B04B5/10Centrifuges combined with other apparatus, e.g. electrostatic separators; Sets or systems of several centrifuges
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K39/00Medicinal preparations containing antigens or antibodies
    • A61K2039/555Medicinal preparations containing antigens or antibodies characterised by a specific combination antigen/adjuvant
    • A61K2039/55505Inorganic adjuvants

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Abstract

A system and a process for producing aluminum hydroxide adjuvant based on an on-line detection and control system relate to the field of vaccine immune adjuvant production, and the system comprises a liquid preparation and supply system, a shearing and mixing system, an aging system, a filtering system, a centrifugal system, a sterilization system, a split charging system and an on-line detection and control system; the liquid preparation and supply system is respectively connected with the shearing and mixing system and the centrifugal system, and the shearing and mixing system, the ageing system, the filtering system, the centrifugal system, the sterilization system and the split charging system are sequentially connected; the on-line detection and control system is respectively arranged in the liquid preparation and supply system, the shearing and mixing system, the aging system, the filtering system and the centrifugal system. Each technological parameter in the preparation process of the aluminum hydroxide adjuvant is monitored and accurately regulated by an online detection and control system of the aluminum hydroxide adjuvant, so that the quality of the aluminum hydroxide adjuvant is accurately controlled; the prepared aluminum hydroxide adjuvant has uniform particle size, stable crystal form, high adsorption efficiency and strong stability, and improves the effectiveness and quality controllability of the aluminum hydroxide adjuvant.

Description

System and process for producing aluminum hydroxide adjuvant based on-line detection and control system
Technical Field
The invention relates to the technical field of vaccine immune adjuvant production, in particular to a system and a process for producing an aluminum hydroxide adjuvant based on an on-line detection and control system.
Background
The aluminum hydroxide gel is used as a medicine slow-release agent, and can achieve larger medicine loading capacity, stable medicine carrying performance and accurate release time control due to the smaller particle size, stable gel performance and complete fiber structure.
The aluminum adjuvant is the most widely used immunological adjuvant at present, and mainly comprises two kinds of aluminum hydroxide and aluminum phosphate, wherein the use of the aluminum hydroxide is wider. The aluminum adjuvant adsorbs antigen through the actions of group exchange, electrostatic attraction, hydrophobic action, van der Waals force, hydrogen bond and the like, so that the effectiveness of the vaccine can be effectively improved, and the action mechanism is that after the aluminum adjuvant adsorbs antigen, the surface area of the antigen is increased, the binding site on the surface of the antigen is fully exposed, the antigen is slowly released, the antigen response is improved, the immunogenicity of the antibody is enhanced, the antibody presentation is stimulated, the cytokine secretion is promoted, the synergistic action of T cells and B cells is enhanced, and the humoral immune response is enhanced. Therefore, the continuous production process of the reinforced aluminum adjuvant, the detection and the refined control of the technological parameters are beneficial to improving the effectiveness and the controllability of the quality of the adjuvant, and further the safety of the aluminum-containing vaccine is ensured. However, no report is made on the production process for guaranteeing the quality of the adjuvant by online detection and automatic regulation of the technological parameters of the production process of the adjuvant.
Disclosure of Invention
In order to improve the effectiveness and quality controllability of the aluminum hydroxide adjuvant, a system and a process for producing the aluminum hydroxide adjuvant based on an on-line detection and control system.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention discloses a system for producing aluminum hydroxide adjuvant based on an on-line detection and control system, which comprises:
the system comprises a liquid preparation and supply system, a shearing and mixing system, an ageing system, a filtering system, a centrifugal system, a sterilization system, a split charging system and an online detection and control system; the liquid preparation and supply system is respectively connected with the shearing and mixing system and the centrifugal system, the shearing and mixing system is connected with the aging system, the aging system is connected with the filtering system, the filtering system is connected with the centrifugal system, the centrifugal system is connected with the sterilizing system, and the sterilizing system is connected with the split charging system; the online detection and control system is respectively arranged in the liquid preparation and supply system, the shearing and mixing system, the aging system, the filtering system and the centrifugal system.
As a preferred embodiment, the online detection and control system includes: the system comprises a concentrated ammonia tank material level online detection system, a concentrated ammonia tank control module, an injection water tank material level online detection system, an injection water tank control module, an ammonia solution tank material level online detection system, an aluminum chloride solution tank control module, a mixing tank multi-parameter online detection system, an aging tank control module, an aging tank multi-parameter online detection system, a concentration tank material level online detection system, a concentration tank control module, a temporary storage tank multi-parameter ion online detection control system and a storage tank multi-parameter ion online detection control system;
The mixing tank multi-parameter online detection system comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
the aging tank multiparameter online detection system comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
the temporary storage tank multiparameter ion online detection control system comprises: the system comprises a temporary storage tank control module, a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
the storage tank multiparameter ion online detection control system comprises: the system comprises a storage tank control module, a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system.
As a preferred embodiment, the liquid preparation and supply system includes: the device comprises a concentrated ammonia water tank, a water tank for injection, a concentrated ammonia water metering pump, a water metering pump for injection, an ammonia water solution tank, a static mixer, an aluminum chloride solution tank, an aluminum chloride metering scale, a sodium chloride tank, a pipeline and a valve; the concentrated ammonia water tank, the concentrated ammonia water metering pump, the static mixer and the ammonia water solution tank are connected with a valve through a pipeline in sequence; the water tank for injection, the metering pump for injection and the aluminum chloride solution tank are connected with a valve through a pipeline in sequence; the metering pump for the water for injection is connected with the static mixer through a pipeline and a valve; the aluminum chloride tank, the aluminum chloride metering scale and the aluminum chloride solution tank are connected with each other through a pipeline and a valve in sequence, and the sodium chloride tank, the sodium chloride metering scale and the aluminum chloride solution tank are connected with each other through a pipeline and a valve in sequence; the online detection system of the material level of the concentrated ammonia water tank and the control module of the concentrated ammonia water tank are arranged on the concentrated ammonia water tank, and the online detection system of the material level of the concentrated ammonia water tank and a liquid inlet valve on the concentrated ammonia water tank are respectively connected with the control module of the concentrated ammonia water tank; the system comprises an injection water tank material level online detection system, an injection water tank control module, a water inlet valve, a water outlet valve, a water inlet valve and a water outlet valve, wherein the injection water tank material level online detection system and the injection water tank control module are arranged on the injection water tank; the ammonia solution tank control module and the ammonia solution tank level online detection system are arranged on the ammonia solution tank, and the ammonia solution tank level online detection system, the concentrated ammonia solution metering pump, the water metering pump for injection, a liquid inlet valve on the ammonia solution tank, a liquid outlet valve on the concentrated ammonia tank and a liquid outlet valve on the water tank for injection are respectively connected with the ammonia solution tank control module; the aluminum chloride solution tank material level online detection system and the aluminum chloride solution tank control module are arranged on the aluminum chloride solution tank, and a liquid outlet valve on the aluminum chloride solution tank material level online detection system and the water tank for injection, a metering pump for injection, an aluminum chloride metering scale, a sodium chloride metering scale and a liquid inlet valve on the aluminum chloride solution tank are respectively connected with the aluminum chloride solution tank control module.
As a preferred embodiment, the shear mixing system comprises: an ammonia water solution metering pump, an aluminum chloride solution metering pump, a shearing pump, a mixing tank, a pipeline and a valve; the ammonia solution tank, the ammonia solution metering pump and the shearing pump are connected with a valve through pipelines in sequence; the aluminum chloride solution tank, the aluminum chloride solution metering pump and the shearing pump are connected with a valve through pipelines in sequence; the shearing pump is connected with the mixing tank through a pipeline and a valve; the multi-parameter on-line detection system of the mixing tank and the control module of the mixing tank are arranged on the mixing tank, and the multi-parameter on-line detection system of the mixing tank, the ammonia water solution metering pump, the aluminum chloride solution metering pump, the shearing pump, the liquid outlet valve on the ammonia water solution tank, the liquid outlet valve on the aluminum chloride solution tank and the liquid inlet valve on the mixing tank are respectively connected with the control module of the mixing tank.
As a preferred embodiment, the aging system comprises: a mixed liquid conveying pump, an aging tank, a pipeline and a valve; the mixing tank, the mixed liquid conveying pump and the aging tank are connected with the valve through pipelines in sequence; the aging tank control module and the aging tank multi-parameter on-line detection system are arranged on the aging tank, and the aging tank multi-parameter on-line detection system, the mixed liquid conveying pump, a liquid outlet valve on the mixing tank and a liquid inlet valve on the aging tank are respectively connected with the aging tank control module.
As a preferred embodiment, the filtration system comprises: an aging tank delivery pump, a filter, a concentration tank, a pipeline and a valve; the aging tank, the aging tank conveying pump, the filter and the concentration tank are connected with the valve through pipelines in sequence; the system is characterized in that the concentration tank material level online detection system and the concentration tank control module are arranged on the concentration tank, and the concentration tank material level online detection system, the aging tank delivery pump, a liquid outlet valve on the aging tank and a liquid inlet valve on the concentration tank are respectively connected with the concentration tank control module.
As a preferred embodiment, the centrifugal system comprises: a concentrating tank conveying pump, a first centrifugal machine, a temporary storage tank, a second centrifugal machine, a storage tank, a waste liquid tank, a pipeline and a valve; the concentrating tank, the concentrating tank conveying pump, the first centrifugal machine, the temporary storage tank, the second centrifugal machine and the storage tank are connected with one another through pipelines and valves in sequence; the centrifugal machine is respectively connected with the concentration tank and the waste liquid tank through pipelines and valves; the two centrifuges are connected with the waste liquid tank through pipelines and valves; the injection water metering pump is connected with the storage tank and the temporary storage tank through pipelines and valves respectively;
the temporary storage tank multiparameter ion online detection control system is arranged on the temporary storage tank, and the injection water metering pump, the centrifugal machine, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system are respectively connected with the temporary storage tank control module;
The storage tank multiparameter ion online detection control system is arranged on the storage tank, and the injection water metering pump, the two-channel centrifugal machine, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system are respectively connected with the storage tank control module.
As a preferred embodiment, the sterilization system comprises: the heat exchanger, the sterilizing tank, the pipeline and the valve are connected in sequence through the pipeline and the valve; the sub-packaging system comprises: sterile filling systems, pipes and valves; the sterilization tank is connected with the sterile filling system through a pipeline and a valve.
The invention relates to a process for producing aluminum hydroxide adjuvant based on an on-line detection and control system, which is realized by adopting the system for producing aluminum hydroxide adjuvant based on the on-line detection and control system, and comprises the following steps:
s1, operating a liquid preparation and supply system;
step S1.1, starting a concentrated ammonia water tank and a concentrated ammonia water metering pump, simultaneously starting an injection water tank and an injection water metering pump, mixing the concentrated ammonia water in the concentrated ammonia water tank and the injection water in the injection water tank in an ammonia water solution tank under the action of a static mixer, and simultaneously starting the stirring function of the ammonia water solution tank to complete the preparation of an ammonia water solution;
S1.2, starting an injection water tank and an injection water metering pump, simultaneously starting an aluminum chloride metering scale, mixing aluminum chloride in the aluminum chloride tank and injection water in the injection water tank in an aluminum chloride solution tank, and simultaneously starting a stirring function of the aluminum chloride solution tank; starting a sodium chloride metering scale, adding sodium chloride into an aluminum chloride solution tank, and completing the preparation of an aluminum chloride solution containing sodium chloride;
when the online detection system of the material level of the concentrated ammonia water tank detects that the liquid level in the concentrated ammonia water tank reaches a low material level, starting a liquid inlet valve on the concentrated ammonia water tank to start feeding through a control module of the concentrated ammonia water tank, and timely supplementing the concentrated ammonia water;
when the on-line detection system of the material level of the injection water tank detects that the liquid level in the injection water tank reaches a low material level, starting a liquid inlet valve on the injection water tank to feed according to a specified proportion through the injection water tank control module, and supplementing injection water in time;
when the online detection system of the material level of the ammonia solution tank detects that the liquid level in the ammonia solution tank reaches a low material level, starting a concentrated ammonia water metering pump, an injection water metering pump, a liquid inlet valve on the ammonia solution tank, a liquid outlet valve on the concentrated ammonia water tank and a liquid outlet valve on the injection water tank through an ammonia solution tank control module to start feeding according to a specified proportion, and timely supplementing concentrated ammonia water and injection water;
When the online detection system of the material level of the aluminum chloride solution tank detects that the liquid level in the aluminum chloride solution tank reaches a low material level, a liquid outlet valve on the injection water tank, an injection water metering pump, an aluminum chloride metering scale, a sodium chloride metering scale and a liquid inlet valve on the aluminum chloride solution tank are started to feed according to a specified proportion by the aluminum chloride solution tank control module, and injection water, aluminum chloride and sodium chloride are timely supplemented;
s2, operating a shearing mixing system;
s2.1, starting an ammonia water solution metering pump and an aluminum chloride solution metering pump, respectively conveying the ammonia water solution in the ammonia water solution tank and the aluminum chloride solution in the aluminum chloride solution tank to a shearing pump, and simultaneously setting the opening of the shearing pump to be 10-60%;
s2.2, feeding the solution obtained by primarily mixing the ammonia water solution and the aluminum chloride solution into a mixing tank, setting the reaction time of the mixing tank to be 30-60min, the reaction temperature to be 58-70 ℃ and the stirring frequency to be 150-500rpm;
when the material level online detection system detects that the liquid level in the mixing tank reaches a low material level, an ammonia water solution metering pump, an aluminum chloride solution metering pump, a shearing pump, a liquid outlet valve on the ammonia water solution tank, a liquid outlet valve on the aluminum chloride solution tank and a liquid inlet valve on the mixing tank are started to feed according to a specified proportion through a mixing tank control module, and the ammonia water solution and the aluminum chloride solution are timely supplemented;
Regulating and controlling the steam flow in the mixing tank through a temperature online detection system so as to control the reaction temperature in the mixing tank, regulating the reaction proportion of ammonia water solution and aluminum chloride solution according to a preset pH value through a pH online detection system, detecting the ion particle size in the mixing tank through a particle size online detection system, detecting the solution viscosity in the mixing tank through a viscosity online detection system, detecting the solution solubility in the mixing tank through a solubility online detection system, and regulating the opening of a shear pump, the reaction time of the mixing tank, the reaction temperature and the stirring frequency according to the preset particle size, the viscosity and the solubility;
s3, operating an aging system;
after the mixing of the ammonia water solution and the aluminum chloride solution is completed, a mixed solution conveying pump is started to convey the mixed solution into an aging tank for aging, and the stirring frequency of the aging tank is 300-500rpm; gradient heating is carried out in an aging tank, 2-3 stages are arranged, gradient heating is carried out at 5-10 ℃/10min in each stage, and heating is stopped and heat is preserved for 10-20min when the temperature of the feed liquid reaches 70 ℃;
detecting the liquid level in the aging tank by using a material level online detection system so as to control the reaction time in the aging tank, and starting a mixed liquid conveying pump, a liquid outlet valve on the mixing tank and a liquid inlet valve on the aging tank to feed by using an aging tank control module when the material level online detection system detects that the liquid level in the aging tank reaches a low material level, so as to timely supplement the mixed liquid;
Regulating and controlling the steam flow in the aging tank through a temperature online detection system so as to control the temperature rising speed and the end temperature in the aging tank, regulating the reaction proportion of the ammonia water solution and the aluminum chloride solution according to a preset pH value through a pH online detection system, detecting the ion particle size in the aging tank through a particle size online detection system, detecting the solution viscosity in the aging tank through a viscosity online detection system, detecting the solution solubility in the aging tank through a solubility online detection system, and regulating the reaction time, the reaction temperature and the stirring frequency of the aging tank according to the preset particle size, the preset viscosity and the preset solubility;
step S4, running the filtering system
Starting an aging tank delivery pump to deliver the aged aluminum hydroxide solution to a filter for filtering, and concentrating the filtered aluminum hydroxide solution in a concentration tank to realize aluminum hydroxide gel separation;
detecting the liquid level in the concentration tank through the concentration tank material level online detection system so as to control the reaction time in the concentration tank, and starting an aging tank conveying pump, a liquid outlet valve on the aging tank and a liquid inlet valve on the concentration tank to feed through a concentration tank control module when the concentration tank material level online detection system detects that the liquid level in the concentration tank reaches a low material level, so as to timely supplement aluminum hydroxide solution;
Step S5, operating the centrifugal system
Starting a conveying pump of a concentration tank to centrifuge the filtered and concentrated aluminum hydroxide solution, wherein two centrifugal separation operations are adopted during centrifugation, one centrifugal operation is firstly carried out by adopting one centrifugal machine, and the solution after the one centrifugal operation is conveyed into a temporary storage tank for temporary storage; then adopting a secondary centrifugal machine to carry out secondary centrifugal operation, and conveying the solution subjected to the secondary centrifugal operation to a storage tank for storage; waste liquid generated by the first centrifugal operation and the second centrifugal operation is conveyed to a waste liquid tank for storage;
detecting the ion content in the temporary storage tank through a multiparameter ion online detection control system of the temporary storage tank, and regulating and controlling the centrifugal speed, the centrifugal time, the centrifugal times and the injection water adding proportion of a centrifugal machine according to the ion content requirement;
detecting the content of aluminum ions in the storage tank by a multi-parameter ion online detection control system of the storage tank, and regulating and controlling the centrifugal speed, the centrifugal time, the centrifugal times and the injection water adding proportion of the two-channel centrifugal machine according to the content requirement of the aluminum ions;
step S6, operating the sterilization system
Conveying the aluminum hydroxide solution in the storage tank to a heat exchanger, heating, conveying to a sterilization tank, starting the sterilization tank for stirring, and performing damp-heat sterilization in the sterilization tank;
Step S7, operating the split charging system
And (5) conveying the aluminum hydroxide solution after the sterilization is qualified to an aseptic filling system, and starting to split into containers.
In the step S5, the centrifugal speed of the centrifugal machine is 3000-6000rpm, the centrifugal time is 30-50min, and the centrifugal is 2-5 times; the stirring time of the temporary storage tank is 10-30min, the stirring frequency is 300-500rpm, and the temporary storage tank circulates for 1-3 times; the centrifugal speed of the secondary centrifugal machine is 3000-6000rpm, the centrifugal time is 30-50min, and the centrifugal is carried out for 2-5 times; the stirring time of the storage tank is 30-60min, the stirring frequency is 300-500rpm, and the temperature is 60+/-2 ℃.
The beneficial effects of the invention are as follows:
according to the system and the process for producing the aluminum hydroxide adjuvant based on the online detection and control system, the aluminum hydroxide adjuvant is prepared by using the ammonia water solution and the aluminum chloride solution, and meanwhile, each technological parameter in the preparation process of the aluminum hydroxide adjuvant is monitored and accurately regulated and controlled through the established online detection and control system of the aluminum hydroxide adjuvant, so that the accurate control of the quality of the aluminum hydroxide adjuvant is realized.
The aluminum hydroxide adjuvant prepared by the process for producing the aluminum hydroxide adjuvant based on the on-line detection and control system is milky colloidal suspension, has uniform particle size, more stable crystal form, higher adsorption efficiency and better stability, and provides powerful guarantee for improving the safety, effectiveness and quality controllability of aluminum-containing vaccines.
Drawings
Fig. 1 is a flow chart of a process for producing aluminum hydroxide adjuvant based on an on-line inspection and control system of the present invention.
In the figure, 1, a concentrated ammonia water tank, 2, a water tank for injection, 3, a concentrated ammonia water metering pump, 4, a water metering pump for injection, 5, an ammonia water solution tank, 6, a static mixer, 7, an ammonia water solution metering pump, 8, an aluminum chloride solution tank, 9, an aluminum chloride tank, 10, an aluminum chloride metering scale, 11, an aluminum chloride solution metering pump, 12, a shearing pump, 13, a mixing tank, 14, a mixing tank control module, 15, a mixed solution delivery pump, 16, an aging tank, 17, an aging tank control module, 18, an aging tank delivery pump, 19, a filter, 20, a concentration tank, 21, a concentration tank delivery pump, 22, one centrifuge, 23, a temporary storage tank, 24, two centrifuges, 25, a storage tank, 26, a heat exchanger, 27, a sterilization tank, 28 and a concentrated ammonia water tank material level online detection system, 29, a mixing tank multiparameter online detection system, 30, an aging tank multiparameter online detection system, 31, a temporary storage tank multiparameter ion online detection control system, 32, a storage tank multiparameter ion online detection control system, 33, an aseptic filling system, 34, a waste liquid tank, 35, a concentrated ammonia tank control module, 36, an injection water tank material level online detection system, 37, an injection water tank control module, 38, an ammonia water tank control module, 39, an ammonia water tank material level online detection system, 40, an aluminum chloride solution tank material level online detection system, 41, an aluminum chloride solution tank control module, 42, a concentration tank material level online detection system, 43, a concentration tank control module, 44, a sodium chloride metering scale, 45 and a sodium chloride tank.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. 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.
As shown in fig. 1, the system for producing aluminum hydroxide adjuvant based on an on-line detection and control system mainly comprises the following subsystems:
the online detection and control system, the liquid preparation and supply system, the shearing and mixing system, the aging system, the filtering system, the centrifugal system, the sterilization system and the split charging system are respectively connected through pipelines and valves. The method comprises the following steps:
the liquid preparation and supply system is respectively connected with the shearing and mixing system and the centrifugal system, the shearing and mixing system is connected with the ageing system, the ageing system is connected with the filtering system, the filtering system is connected with the centrifugal system, the centrifugal system is connected with the sterilizing system, and the sterilizing system is connected with the split charging system;
The online detection and control system is respectively arranged in the liquid preparation and supply system, the shearing and mixing system, the aging system, the filtering system and the centrifugal system; the on-line detection and control system specifically comprises: the system comprises a concentrated ammonia tank material level online detection system 28, a concentrated ammonia tank control module 35, an injection water tank material level online detection system 36, an injection water tank control module 37, an ammonia solution tank control module 38, an ammonia solution tank material level online detection system 39, an aluminum chloride solution tank material level online detection system 40, an aluminum chloride solution tank control module 41, a mixing tank control module 14, a mixing tank multi-parameter online detection system 29, an aging tank control module 17, an aging tank multi-parameter online detection system 30, a concentration tank material level online detection system 42, a concentration tank control module 43, a temporary storage tank multi-parameter ion online detection control system 31 and a storage tank multi-parameter ion online detection control system 32;
the liquid preparation and supply system mainly comprises: a concentrated ammonia water tank 1, a water tank 2 for injection, a concentrated ammonia water metering pump 3, a water metering pump 4 for injection, an ammonia water solution tank 5, a static mixer 6, an aluminum chloride solution tank 8, an aluminum chloride tank 9, an aluminum chloride metering scale 10, a sodium chloride metering scale 44, a sodium chloride tank 45, a pipeline and a valve; the concentrated ammonia water tank 1, the concentrated ammonia water metering pump 3, the static mixer 6 and the ammonia water solution tank 5 are connected with a valve through pipelines in sequence; the water tank 2 for injection, the metering pump 4 for injection and the aluminum chloride solution tank 8 are connected with a valve through a pipeline in sequence; the injection water metering pump 4 and the static mixer 6 are connected through a pipeline and a valve; the aluminum chloride tank 9, the aluminum chloride metering scale 10 and the aluminum chloride solution tank 8 are connected with each other through pipelines and valves in sequence, and the sodium chloride tank 45, the sodium chloride metering scale 44 and the aluminum chloride solution tank 8 are connected with each other through pipelines and valves in sequence; the system comprises a concentrated ammonia water tank 1, a concentrated ammonia water tank control module 35, a concentrated ammonia water tank material level online detection system 28, a concentrated ammonia water tank control module 35 and a concentrated ammonia water tank 1, wherein the concentrated ammonia water tank material level online detection system 28 and the concentrated ammonia water tank 1 are respectively connected with liquid inlet valves; the injection water tank 2 is provided with an injection water tank material level online detection system 36 and an injection water tank control module 37, the injection water tank material level online detection system 36 and a liquid inlet valve on the injection water tank 2 are respectively connected with the injection water tank control module 37, and the injection water tank control module 37 can control the injection water tank material level online detection system 36 and the liquid inlet valve on the injection water tank 2 to work according to requirements; the ammonia solution tank 5 is provided with an ammonia solution tank control module 38 and an ammonia solution tank material level online detection system 39, the ammonia solution tank material level online detection system 39, a concentrated ammonia water metering pump 3, an injection water metering pump 4, a liquid inlet valve on the ammonia solution tank 5, a liquid outlet valve on the concentrated ammonia water tank 1 and a liquid outlet valve on the injection water tank 2 are respectively connected with the ammonia solution tank control module 38, and the ammonia solution tank material level online detection system 39, the concentrated ammonia water metering pump 3, the injection water metering pump 4, the liquid inlet valve on the ammonia solution tank 5, the liquid outlet valve on the concentrated ammonia water tank 1 and the liquid outlet valve on the injection water tank 2 can be controlled by the ammonia solution tank control module 38 to work according to requirements; the aluminum chloride solution tank 8 is provided with an aluminum chloride solution tank material level online detection system 40 and an aluminum chloride solution tank control module 41, wherein a liquid outlet valve on the aluminum chloride solution tank 40, a water injection metering pump 4, an aluminum chloride metering scale 10, a sodium chloride metering scale 44 and a liquid inlet valve on the aluminum chloride solution tank 8 are respectively connected with the aluminum chloride solution tank control module 41, and the aluminum chloride solution tank control module 41 can control the liquid outlet valve on the aluminum chloride solution tank material level online detection system 40, the water injection metering pump 4, the aluminum chloride metering scale 10, the sodium chloride metering scale 44 and the liquid inlet valve on the aluminum chloride solution tank 8 to work according to requirements;
The shear mixing system mainly comprises: an ammonia water solution metering pump 7, an aluminum chloride solution metering pump 11, a shearing pump 12, a mixing tank 13, a pipeline and a valve; the ammonia solution tank 5, the ammonia solution metering pump 7 and the shearing pump 12 are connected with a valve through pipelines in sequence; the aluminum chloride solution tank 8, the aluminum chloride solution metering pump 11 and the shearing pump 12 are connected with a valve through pipelines in sequence; the shear pump 12 and the mixing tank 13 are connected through a pipeline and a valve; the mixing tank 13 is provided with a mixing tank multi-parameter on-line detection system 29 and a mixing tank control module 14, the mixing tank multi-parameter on-line detection system 29, an ammonia solution metering pump 7, an aluminum chloride solution metering pump 11, a shear pump 12, a liquid outlet valve on the ammonia solution tank 5, a liquid outlet valve on the aluminum chloride solution tank 8 and a liquid inlet valve on the mixing tank 13 are respectively connected with the mixing tank control module 14, and the mixing tank control module 14 can control the mixing tank multi-parameter on-line detection system 29, the ammonia solution metering pump 7, the aluminum chloride solution metering pump 11, the shear pump 12, the liquid outlet valve on the ammonia solution tank 5, the liquid outlet valve on the aluminum chloride solution tank 8 and the liquid inlet valve on the mixing tank 13 to work according to requirements; the mixing tank multi-parameter on-line detection system 29 mainly comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
The aging system mainly comprises: a mixed liquor delivery pump 15, an aging tank 16, a pipeline and a valve; the mixing tank 13, the mixed liquid delivery pump 15 and the aging tank 16 are connected with a valve through pipelines in sequence; the ageing tank 16 is provided with an ageing tank control module 17 and an ageing tank multi-parameter online detection system 30, the ageing tank multi-parameter online detection system 30, a mixed liquid delivery pump 15, a liquid outlet valve on the mixed tank 13 and a liquid inlet valve on the ageing tank 16 are respectively connected with the ageing tank control module 17, and the ageing tank multi-parameter online detection system 30, the mixed liquid delivery pump 15, the liquid outlet valve on the mixed tank 13 and the liquid inlet valve on the ageing tank 16 can be controlled by the ageing tank control module 17 to work according to requirements; the aging tank multiparameter online detection system 30 mainly comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
the filtering system mainly comprises: an aging tank conveying pump 18, a filter 19, a concentration tank 20, pipelines and valves; the ageing tank 16, the ageing tank conveying pump 18, the filter 19 and the concentration tank 20 are connected with valves through pipelines in sequence; the concentration tank 20 is provided with a concentration tank material level online detection system 42 and a concentration tank control module 43, the concentration tank material level online detection system 42, the aging tank delivery pump 18, a liquid outlet valve on the aging tank 16 and a liquid inlet valve on the concentration tank 20 are respectively connected with the concentration tank control module 43, and the concentration tank material level online detection system 42, the aging tank delivery pump 18, the liquid outlet valve on the aging tank 16 and the liquid inlet valve on the concentration tank 20 can be controlled to work according to requirements through the concentration tank control module 43; in the present embodiment, the filter 19 may be a plate type airtight filter, but is not limited thereto;
The centrifugal system mainly comprises: a concentrating tank conveying pump 21, a centrifugal machine 22, a temporary storage tank 23, a centrifugal machine 24, a storage tank 25, a waste liquid tank 34, pipelines and valves; the concentration tank 20, the concentration tank delivery pump 21, the first centrifugal machine 22, the temporary storage tank 23, the second centrifugal machine 24 and the storage tank 25 are connected in sequence through pipelines and valves; a centrifuge 22 is connected to the concentrate tank 20 and the waste liquid tank 34 by pipes and valves, respectively; the secondary centrifuge 24 is connected with the waste liquid tank 34 through a pipeline and a valve; the metering pump 4 for injection is respectively connected with the storage tank 25 and the temporary storage tank 23 through pipelines and valves;
wherein, the temporary storage tank 23 is provided with a temporary storage tank multiparameter ion online detection control system 31, and the temporary storage tank multiparameter ion online detection control system 31 mainly comprises: the system comprises a temporary storage tank control module, a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system; the water metering pump 4 for injection, the centrifugal machine 22, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system are respectively connected with a temporary storage tank control module, and the water metering pump 4 for injection, the centrifugal machine 22, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system can be controlled to work according to requirements through the temporary storage tank control module;
The storage tank 25 is provided with a storage tank multiparameter ion online detection control system 32, and the storage tank multiparameter ion online detection control system 32 mainly comprises: the system comprises a storage tank control module, a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system; the water metering pump 4 for injection, the two-channel centrifugal machine 24, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system are respectively connected with the storage tank control module; the water metering pump 4 for injection, the secondary centrifuge 24, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system can be controlled to work according to requirements through the storage tank control module;
the sterilization system mainly comprises: a heat exchanger 26, a sterilization tank 27, a pipeline and a valve; the storage tank 25, the heat exchanger 26 and the sterilization tank 27 are connected with a valve through pipelines in sequence;
the split charging system mainly comprises: sterile filling system 33, tubing and valves; the sterilization tank 27 and the sterile filling system 33 are connected by piping and valves.
As shown in fig. 1, the process for producing aluminum hydroxide adjuvant based on the on-line inspection and control system is realized by adopting the system for producing aluminum hydroxide adjuvant based on the on-line inspection and control system, and specifically comprises the following steps:
s1, operating a liquid preparation and supply system;
step S1.1, firstly preparing an ammonia water solution, starting a concentrated ammonia water tank 1 and a concentrated ammonia water metering pump 3, simultaneously starting an injection water tank 2 and an injection water metering pump 4, mixing the concentrated ammonia water in the concentrated ammonia water tank 1 and the injection water in the injection water tank 2 in an ammonia water solution tank 5 under the action of a static mixer 6, and simultaneously starting the stirring function of the ammonia water solution tank 5, and diluting the concentrated ammonia water according to a certain proportion, thereby completing the preparation of the ammonia water solution;
as a preferred embodiment, the concentrated aqueous ammonia and the water for injection are uniformly mixed in a ratio of 1:3 (V: V) at the time of diluting the concentrated aqueous ammonia, but not limited thereto;
step S1.2, preparing an aluminum chloride solution, starting an injection water tank 2 and an injection water metering pump 4, simultaneously starting an aluminum chloride metering scale 10, mixing aluminum chloride in an aluminum chloride tank 9 and injection water in the injection water tank 2 in an aluminum chloride solution tank 8, and simultaneously starting a stirring function of the aluminum chloride solution tank 8; starting a sodium chloride metering scale 44, adding sodium chloride into the aluminum chloride solution tank 8, and preparing an aluminum chloride solution according to a certain proportion, thereby completing the preparation of the aluminum chloride solution containing sodium chloride;
As a preferred embodiment, when preparing the aluminum chloride solution, aluminum chloride and water for injection are uniformly mixed according to the proportion of 1g to 24mL (M: V), but the method is not limited to the method;
because the concentrated ammonia water tank 1 is provided with the concentrated ammonia water tank material level online detection system 28 and the concentrated ammonia water tank control module 35, the injection water tank 2 is provided with the injection water tank material level online detection system 36 and the injection water tank control module 37, the ammonia water solution tank 5 is provided with the ammonia water solution tank control module 38 and the ammonia water solution tank material level online detection system 39, and the aluminum chloride solution tank 8 is provided with the aluminum chloride solution tank material level online detection system 40 and the aluminum chloride solution tank control module 41; thus, the liquid level in the concentrated ammonia water tank 1 can be detected by the concentrated ammonia water tank level online detection system 28, the liquid level in the water tank for injection 2 can be detected by the water tank for injection level online detection system 36, the liquid level in the aqueous ammonia solution tank 5 can be detected by the aqueous ammonia solution tank level online detection system 39, and the liquid level in the aluminum chloride solution tank 8 can be detected by the aluminum chloride solution tank level online detection system 40; when the liquid level in the concentrated ammonia water tank 1, the water tank 2 for injection, the ammonia water solution tank 5 or the aluminum chloride solution tank 8 reaches a low material level, corresponding pumps and valves can be started through corresponding control modules, so that feeding is performed according to a specified proportion, and liquid preparation is timely supplemented; the method comprises the following steps:
When the online detection system 28 of the material level of the concentrated ammonia water tank detects that the liquid level in the concentrated ammonia water tank 1 reaches a low material level, a liquid inlet valve on the concentrated ammonia water tank 1 is started to start feeding through the control module 35 of the concentrated ammonia water tank, and the concentrated ammonia water is timely supplemented;
when the on-line detection system 36 of the material level of the water tank for injection detects that the liquid level in the water tank for injection 2 reaches a low material level, the water tank for injection control module 37 starts a liquid inlet valve on the water tank for injection 2 to start feeding according to a specified proportion, and the water for injection is timely replenished;
when the online ammonia solution tank level detection system 39 detects that the liquid level in the ammonia solution tank 5 reaches a low level, starting the concentrated ammonia solution metering pump 3, the water injection metering pump 4, a liquid inlet valve on the ammonia solution tank 5, a liquid outlet valve on the concentrated ammonia water tank 1 and a liquid outlet valve on the water injection tank 2 through the ammonia solution tank control module 38 to start feeding according to a specified proportion, and timely supplementing concentrated ammonia water and water injection;
when the online detection system 40 of the material level of the aluminum chloride solution tank detects that the liquid level in the aluminum chloride solution tank 8 reaches a low material level, a liquid outlet valve on the water tank 2 for injection, the metering pump 4 for injection, the aluminum chloride metering scale 10, the sodium chloride metering scale 44 and a liquid inlet valve on the aluminum chloride solution tank 8 are started to feed according to a specified proportion by the control module 41 of the aluminum chloride solution tank, and water for injection, aluminum chloride and sodium chloride are timely supplemented;
S2, operating a shearing mixing system;
the shear mixing system functions as: accurately mixing two basic solutions of an ammonia water solution and an aluminum chloride solution according to a certain proportion, and simultaneously realizing the generation of aluminum hydroxide by controlling the process parameters of reaction time, reaction temperature, stirring frequency, opening of a shearing pump 12 and the like of a mixing tank 13;
the method comprises the following specific steps:
s2.1, simultaneously starting an ammonia water solution metering pump 7 and an aluminum chloride solution metering pump 11, respectively conveying the ammonia water solution in an ammonia water solution tank 5 and the aluminum chloride solution in an aluminum chloride solution tank 8 to a shearing pump 12 according to a certain proportion, and simultaneously setting the opening of the shearing pump 12;
as a preferred embodiment, the opening of the shear pump 12 is set to 10 to 60%;
step S2.2, feeding the solution obtained by primarily mixing the ammonia water solution and the aluminum chloride solution into a mixing tank 13, and setting the reaction time, the reaction temperature and the stirring frequency of the mixing tank 13;
as a preferred embodiment, the reaction time of the mixing tank 13 is 30-60min, the reaction temperature is 58-70 ℃ and the stirring frequency is 150-500rpm;
the mixing tank 13 is provided with a mixing tank multi-parameter on-line detection system 29 and a mixing tank control module 14, wherein the mixing tank multi-parameter on-line detection system 29 mainly comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system; therefore, the liquid level in the mixing tank 13 can be detected by the material level on-line detection system, so that the reaction time in the mixing tank 13 can be controlled, and in addition, when the material level on-line detection system detects that the liquid level in the mixing tank 13 reaches a low material level, the ammonia water solution metering pump 7, the aluminum chloride solution metering pump 11, the shearing pump 12, a liquid outlet valve on the ammonia water solution tank 5, a liquid outlet valve on the aluminum chloride solution tank 8 and a liquid inlet valve on the mixing tank 13 are started to feed according to a specified proportion, so that the ammonia water solution and the aluminum chloride solution are timely supplemented; the steam flow in the mixing tank 13 can be regulated and controlled through a temperature online detection system, the reaction temperature in the mixing tank 13 can be further controlled, the reaction proportion of the ammonia water solution and the aluminum chloride solution is regulated according to a preset pH value through a pH online detection system, the ion particle size in the mixing tank 13 is detected through a particle size online detection system, the solution viscosity in the mixing tank 13 is detected through a viscosity online detection system, the solution solubility in the mixing tank 13 is detected through a solubility online detection system, the opening of the shear pump 12 and the reaction time, the reaction temperature and the stirring frequency of the mixing tank 13 can be regulated according to three preset parameter values (particle size, viscosity and solubility), and meanwhile, the proportion and the sequence of the response values of the three parameters (particle size, viscosity and solubility) can be regulated according to requirements;
S3, operating an aging system;
the ageing system has the functions of: after the mixing reaction of the ammonia water solution and the aluminum chloride solution is finished, the formation of the crystal form of the aluminum hydroxide adjuvant is promoted, and the stability of the aluminum hydroxide adjuvant is improved;
the method comprises the following specific steps:
after the mixing of the ammonia water solution and the aluminum chloride solution is completed, a mixed solution conveying pump 15 is started to convey the mixed solution into an aging tank 16 for aging;
as a preferred embodiment, when the ageing tank 16 is used for ageing, the material liquid needs to be controlled to be subjected to gradient heating, the process can be provided with 2-3 stages, the gradient heating is carried out at 5-10 ℃/10min in each stage, when the material liquid temperature reaches 70 ℃, the heating is stopped and the temperature is kept for 10-20min, and the stirring frequency of the ageing tank 16 is 300-500rpm;
the aging tank 16 is provided with an aging tank control module 17 and an aging tank multi-parameter online detection system 30, wherein the aging tank multi-parameter online detection system 30 mainly comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system; therefore, the liquid level in the aging tank 16 can be detected by the material level on-line detection system, so that the reaction time in the aging tank 16 can be controlled, and in addition, when the material level on-line detection system detects that the liquid level in the aging tank 16 reaches a low material level, the mixed liquid conveying pump 15, a liquid outlet valve on the mixing tank 13 and a liquid inlet valve on the aging tank 16 are started by the aging tank control module 17 to start feeding, so that mixed liquid is timely supplemented; the steam flow in the aging tank 16 can be regulated and controlled through a temperature online detection system, the heating speed and the end temperature in the aging tank 16 can be further controlled, the reaction proportion of the ammonia water solution and the aluminum chloride solution can be regulated according to a preset pH value through a pH online detection system, the ion particle size in the aging tank 16 is detected through a particle size online detection system, the solution viscosity in the aging tank 16 is detected through a viscosity online detection system, the solution solubility in the aging tank 16 is detected through a solubility online detection system, the regulation of the reaction time, the reaction temperature and the stirring frequency of the aging tank 16 can be realized according to three preset parameter values (particle size, viscosity and solubility), and meanwhile, the proportion and the sequence of the response values of three parameters (particle size, viscosity and solubility) can be regulated according to requirements;
Step S4, running the filtering system
After the aging is finished, an aging tank conveying pump 18 is started to convey the aged aluminum hydroxide solution into a filter 19 for filtering, and the filtered aluminum hydroxide solution enters a concentration tank 20 for concentration, so that aluminum hydroxide gel separation is realized;
the concentration tank 20 is provided with a concentration tank material level on-line detection system 42 and a concentration tank control module 43, the liquid level in the concentration tank 20 can be detected by the concentration tank material level on-line detection system 42 so as to control the reaction time in the concentration tank 20, in addition, when the concentration tank material level on-line detection system 42 detects that the liquid level in the concentration tank 20 reaches a low material level, the concentration tank control module 43 starts the ageing tank conveying pump 18, a liquid outlet valve on the ageing tank 16 and a liquid inlet valve on the concentration tank 20 to start feeding, and the aluminum hydroxide solution is timely replenished;
step S5, operating the centrifugal system
After the filtration is completed, a concentration tank conveying pump 21 is started to centrifuge the filtered and concentrated aluminum hydroxide solution, two centrifugal separation operations are adopted during the centrifugation, one centrifugal operation is firstly carried out by adopting a centrifugal machine 22, and the solution after the one centrifugal operation is conveyed to a temporary storage tank 23 for temporary storage; then adopting a secondary centrifugal machine 24 to carry out secondary centrifugal operation, and conveying the solution subjected to the secondary centrifugal operation to a storage tank 25 for storage; the waste liquid generated by the first centrifugal operation and the second centrifugal operation is conveyed to a waste liquid tank 34 for storage;
As a preferred embodiment, during one centrifugation operation, the centrifugal speed of one centrifuge 22 is 3000-6000rpm, the centrifugal time is 30-50min, and the centrifugation is 2-5 times;
as a preferable implementation mode, a temporary storage tank 23 is arranged after the centrifugal machine 22, the stirring time of the temporary storage tank 23 is 10-30min, the stirring frequency is 300-500rpm, and the temporary storage tank is circulated for 1-3 times;
as a preferred implementation mode, during the secondary centrifugal operation, the centrifugal speed of the secondary centrifugal machine 24 is 3000-6000rpm, the centrifugal time is 30-50min, and the centrifugal is 2-5 times;
as a preferred embodiment, the storage tank 25 is arranged after the two-channel centrifugal machine 24, the stirring time of the storage tank 25 is 30-60min, the stirring frequency is 300-500rpm, and the temperature is 60+/-2 ℃;
the temporary storage tank 23 is provided with a temporary storage tank multiparameter ion online detection control system 31, and the temporary storage tank multiparameter ion online detection control system 31 is used for detecting the ion content in the temporary storage tank 23 and further regulating and controlling the centrifugal speed, the centrifugal time, the centrifugal times and the injection water adding proportion of the centrifugal machine 22 according to the ion content requirement;
the storage tank 25 is provided with a storage tank multiparameter ion online detection control system 32, and the storage tank multiparameter ion online detection control system 32 is used for detecting the content of aluminum ions in the storage tank 25 and further regulating and controlling the centrifugal speed, the centrifugal time, the centrifugal times and the injection water adding proportion of the two-channel centrifugal machine 24 according to the content requirement of the aluminum ions;
Step S6, operating the sterilization system
Delivering the qualified aluminum hydroxide solution in the storage tank 25 to a heat exchanger 26, heating, delivering the aluminum hydroxide solution to a sterilization tank 27, starting the sterilization tank 27 for stirring, and performing damp-heat sterilization in the sterilization tank 27;
step S7, operating the split charging system
The aluminum hydroxide solution after passing the sterilization is sent to a sterile filling system 33, and the aluminum hydroxide solution starts to be packaged in containers.
The invention discloses a system and a process for producing an aluminum hydroxide adjuvant based on an on-line detection and control system, and a person skilled in the art can refer to the content of the invention to properly improve the process parameters. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the invention has been described with reference to preferred embodiments, it will be apparent to those skilled in the relevant art that variations and modifications can be made in the invention described herein without departing from the spirit or scope of the invention.

Claims (3)

1. A system for producing an aluminum hydroxide adjuvant based on an on-line inspection and control system, comprising: the system comprises a liquid preparation and supply system, a shearing and mixing system, an ageing system, a filtering system, a centrifugal system, a sterilization system, a split charging system and an online detection and control system; the liquid preparation and supply system is respectively connected with the shearing and mixing system and the centrifugal system, the shearing and mixing system is connected with the aging system, the aging system is connected with the filtering system, the filtering system is connected with the centrifugal system, the centrifugal system is connected with the sterilizing system, and the sterilizing system is connected with the split charging system; the online detection and control system is respectively arranged in the liquid preparation and supply system, the shearing and mixing system, the aging system, the filtering system and the centrifugal system;
The online detection and control system comprises: the system comprises a concentrated ammonia tank material level online detection system, a concentrated ammonia tank control module, an injection water tank material level online detection system, an injection water tank control module, an ammonia solution tank material level online detection system, an aluminum chloride solution tank control module, a mixing tank multi-parameter online detection system, an aging tank control module, an aging tank multi-parameter online detection system, a concentration tank material level online detection system, a concentration tank control module, a temporary storage tank multi-parameter ion online detection control system and a storage tank multi-parameter ion online detection control system;
the mixing tank multi-parameter online detection system comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
the aging tank multiparameter online detection system comprises: the system comprises a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
The temporary storage tank multiparameter ion online detection control system comprises: the system comprises a temporary storage tank control module, a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
the storage tank multiparameter ion online detection control system comprises: the system comprises a storage tank control module, a material level online detection system, a temperature online detection system, a pH online detection system, a particle size online detection system, a viscosity online detection system and a solubility online detection system;
the liquid preparation and supply system comprises: the device comprises a concentrated ammonia water tank, a water tank for injection, a concentrated ammonia water metering pump, a water metering pump for injection, an ammonia water solution tank, a static mixer, an aluminum chloride solution tank, an aluminum chloride metering scale, a sodium chloride tank, a pipeline and a valve; the concentrated ammonia water tank, the concentrated ammonia water metering pump, the static mixer and the ammonia water solution tank are connected with a valve through a pipeline in sequence; the water tank for injection, the metering pump for injection and the aluminum chloride solution tank are connected with a valve through a pipeline in sequence; the metering pump for the water for injection is connected with the static mixer through a pipeline and a valve; the aluminum chloride tank, the aluminum chloride metering scale and the aluminum chloride solution tank are connected with each other through a pipeline and a valve in sequence, and the sodium chloride tank, the sodium chloride metering scale and the aluminum chloride solution tank are connected with each other through a pipeline and a valve in sequence; the online detection system of the material level of the concentrated ammonia water tank and the control module of the concentrated ammonia water tank are arranged on the concentrated ammonia water tank, and the online detection system of the material level of the concentrated ammonia water tank and a liquid inlet valve on the concentrated ammonia water tank are respectively connected with the control module of the concentrated ammonia water tank; the system comprises an injection water tank material level online detection system, an injection water tank control module, a water inlet valve, a water outlet valve, a water inlet valve and a water outlet valve, wherein the injection water tank material level online detection system and the injection water tank control module are arranged on the injection water tank; the ammonia solution tank control module and the ammonia solution tank level online detection system are arranged on the ammonia solution tank, and the ammonia solution tank level online detection system, the concentrated ammonia solution metering pump, the water metering pump for injection, a liquid inlet valve on the ammonia solution tank, a liquid outlet valve on the concentrated ammonia tank and a liquid outlet valve on the water tank for injection are respectively connected with the ammonia solution tank control module; the aluminum chloride solution tank material level online detection system and the aluminum chloride solution tank control module are arranged on the aluminum chloride solution tank, and the aluminum chloride solution tank material level online detection system, a liquid outlet valve on the water tank for injection, a metering pump for injection, an aluminum chloride metering scale, a sodium chloride metering scale and a liquid inlet valve on the aluminum chloride solution tank are respectively connected with the aluminum chloride solution tank control module;
The shear mixing system includes: an ammonia water solution metering pump, an aluminum chloride solution metering pump, a shearing pump, a mixing tank, a pipeline and a valve; the ammonia solution tank, the ammonia solution metering pump and the shearing pump are connected with a valve through pipelines in sequence; the aluminum chloride solution tank, the aluminum chloride solution metering pump and the shearing pump are connected with a valve through pipelines in sequence; the shearing pump is connected with the mixing tank through a pipeline and a valve; the multi-parameter on-line detection system of the mixing tank and the control module of the mixing tank are arranged on the mixing tank, and the multi-parameter on-line detection system of the mixing tank, the ammonia water solution metering pump, the aluminum chloride solution metering pump, the shearing pump, a liquid outlet valve on the ammonia water solution tank, a liquid outlet valve on the aluminum chloride solution tank and a liquid inlet valve on the mixing tank are respectively connected with the control module of the mixing tank;
the aging system comprises: a mixed liquid conveying pump, an aging tank, a pipeline and a valve; the mixing tank, the mixed liquid conveying pump and the aging tank are connected with the valve through pipelines in sequence; the aging tank control module and the aging tank multi-parameter on-line detection system are arranged on the aging tank, and the aging tank multi-parameter on-line detection system, the mixed liquid conveying pump, a liquid outlet valve on the mixing tank and a liquid inlet valve on the aging tank are respectively connected with the aging tank control module;
The filtration system comprises: an aging tank delivery pump, a filter, a concentration tank, a pipeline and a valve; the aging tank, the aging tank conveying pump, the filter and the concentration tank are connected with the valve through pipelines in sequence; the system comprises a concentration tank material level online detection system, an aging tank conveying pump, a liquid outlet valve on the aging tank and a liquid inlet valve on the concentration tank, wherein the concentration tank material level online detection system and the concentration tank control module are arranged on the concentration tank;
the centrifugal system comprises: a concentrating tank conveying pump, a first centrifugal machine, a temporary storage tank, a second centrifugal machine, a storage tank, a waste liquid tank, a pipeline and a valve; the concentrating tank, the concentrating tank conveying pump, the first centrifugal machine, the temporary storage tank, the second centrifugal machine and the storage tank are connected with one another through pipelines and valves in sequence; the centrifugal machine is respectively connected with the concentration tank and the waste liquid tank through pipelines and valves; the two centrifuges are connected with the waste liquid tank through pipelines and valves; the injection water metering pump is connected with the storage tank and the temporary storage tank through pipelines and valves respectively;
the temporary storage tank multiparameter ion online detection control system is arranged on the temporary storage tank, and the injection water metering pump, the centrifugal machine, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system are respectively connected with the temporary storage tank control module;
The storage tank multiparameter ion online detection control system is arranged on the storage tank, and the injection water metering pump, the two-channel centrifugal machine, the material level online detection system, the temperature online detection system, the pH online detection system, the particle size online detection system, the viscosity online detection system and the solubility online detection system are respectively connected with the storage tank control module;
the sterilization system includes: the heat exchanger, the sterilizing tank, the pipeline and the valve are connected in sequence through the pipeline and the valve; the sub-packaging system comprises: sterile filling systems, pipes and valves; the sterilization tank is connected with the sterile filling system through a pipeline and a valve.
2. A process for producing aluminum hydroxide adjuvant based on an on-line inspection and control system, which is characterized in that the system for producing aluminum hydroxide adjuvant based on the on-line inspection and control system is realized by adopting the system for producing aluminum hydroxide adjuvant based on the on-line inspection and control system as claimed in claim 1, and comprises the following steps:
s1, operating a liquid preparation and supply system;
step S1.1, starting a concentrated ammonia water tank and a concentrated ammonia water metering pump, simultaneously starting an injection water tank and an injection water metering pump, mixing the concentrated ammonia water in the concentrated ammonia water tank and the injection water in the injection water tank in an ammonia water solution tank under the action of a static mixer, and simultaneously starting the stirring function of the ammonia water solution tank to complete the preparation of an ammonia water solution;
S1.2, starting an injection water tank and an injection water metering pump, simultaneously starting an aluminum chloride metering scale, mixing aluminum chloride in the aluminum chloride tank and injection water in the injection water tank in an aluminum chloride solution tank, and simultaneously starting a stirring function of the aluminum chloride solution tank; starting a sodium chloride metering scale, adding sodium chloride into an aluminum chloride solution tank, and completing the preparation of an aluminum chloride solution containing sodium chloride;
when the online detection system of the material level of the concentrated ammonia water tank detects that the liquid level in the concentrated ammonia water tank reaches a low material level, starting a liquid inlet valve on the concentrated ammonia water tank to start feeding through a control module of the concentrated ammonia water tank, and timely supplementing the concentrated ammonia water;
when the on-line detection system of the material level of the injection water tank detects that the liquid level in the injection water tank reaches a low material level, starting a liquid inlet valve on the injection water tank to feed according to a specified proportion through the injection water tank control module, and supplementing injection water in time;
when the online detection system of the material level of the ammonia solution tank detects that the liquid level in the ammonia solution tank reaches a low material level, starting a concentrated ammonia water metering pump, an injection water metering pump, a liquid inlet valve on the ammonia solution tank, a liquid outlet valve on the concentrated ammonia water tank and a liquid outlet valve on the injection water tank through an ammonia solution tank control module to start feeding according to a specified proportion, and timely supplementing concentrated ammonia water and injection water;
When the online detection system of the material level of the aluminum chloride solution tank detects that the liquid level in the aluminum chloride solution tank reaches a low material level, a liquid outlet valve on the injection water tank, an injection water metering pump, an aluminum chloride metering scale, a sodium chloride metering scale and a liquid inlet valve on the aluminum chloride solution tank are started to feed according to a specified proportion by the aluminum chloride solution tank control module, and injection water, aluminum chloride and sodium chloride are timely supplemented;
s2, operating a shearing mixing system;
s2.1, starting an ammonia water solution metering pump and an aluminum chloride solution metering pump, respectively conveying the ammonia water solution in the ammonia water solution tank and the aluminum chloride solution in the aluminum chloride solution tank to a shearing pump, and simultaneously setting the opening of the shearing pump to be 10-60%;
s2.2, feeding the solution obtained by primarily mixing the ammonia water solution and the aluminum chloride solution into a mixing tank, setting the reaction time of the mixing tank to be 30-60min, the reaction temperature to be 58-70 ℃ and the stirring frequency to be 150-500rpm;
when the material level online detection system detects that the liquid level in the mixing tank reaches a low material level, an ammonia water solution metering pump, an aluminum chloride solution metering pump, a shearing pump, a liquid outlet valve on the ammonia water solution tank, a liquid outlet valve on the aluminum chloride solution tank and a liquid inlet valve on the mixing tank are started to feed according to a specified proportion through a mixing tank control module, and the ammonia water solution and the aluminum chloride solution are timely supplemented;
Regulating and controlling the steam flow in the mixing tank through a temperature online detection system so as to control the reaction temperature in the mixing tank, regulating the reaction proportion of ammonia water solution and aluminum chloride solution according to a preset pH value through a pH online detection system, detecting the ion particle size in the mixing tank through a particle size online detection system, detecting the solution viscosity in the mixing tank through a viscosity online detection system, detecting the solution solubility in the mixing tank through a solubility online detection system, and regulating the opening of a shear pump, the reaction time of the mixing tank, the reaction temperature and the stirring frequency according to the preset particle size, the viscosity and the solubility;
s3, operating an aging system;
after the mixing of the ammonia water solution and the aluminum chloride solution is completed, a mixed solution conveying pump is started to convey the mixed solution into an aging tank for aging, and the stirring frequency of the aging tank is 300-500rpm; gradient heating is carried out in an aging tank, 2-3 stages are arranged, gradient heating is carried out at 5-10 ℃/10min in each stage, and heating is stopped and heat is preserved for 10-20min when the temperature of the feed liquid reaches 70 ℃;
detecting the liquid level in the aging tank by using a material level online detection system so as to control the reaction time in the aging tank, and starting a mixed liquid conveying pump, a liquid outlet valve on the mixing tank and a liquid inlet valve on the aging tank to feed by using an aging tank control module when the material level online detection system detects that the liquid level in the aging tank reaches a low material level, so as to timely supplement the mixed liquid;
Regulating and controlling the steam flow in the aging tank through a temperature online detection system so as to control the temperature rising speed and the end temperature in the aging tank, regulating the reaction proportion of the ammonia water solution and the aluminum chloride solution according to a preset pH value through a pH online detection system, detecting the ion particle size in the aging tank through a particle size online detection system, detecting the solution viscosity in the aging tank through a viscosity online detection system, detecting the solution solubility in the aging tank through a solubility online detection system, and regulating the reaction time, the reaction temperature and the stirring frequency of the aging tank according to the preset particle size, the preset viscosity and the preset solubility;
step S4, running the filtering system
Starting an aging tank delivery pump to deliver the aged aluminum hydroxide solution to a filter for filtering, and concentrating the filtered aluminum hydroxide solution in a concentration tank to realize aluminum hydroxide gel separation;
detecting the liquid level in the concentration tank through the concentration tank material level online detection system so as to control the reaction time in the concentration tank, and starting an aging tank conveying pump, a liquid outlet valve on the aging tank and a liquid inlet valve on the concentration tank to feed through a concentration tank control module when the concentration tank material level online detection system detects that the liquid level in the concentration tank reaches a low material level, so as to timely supplement aluminum hydroxide solution;
Step S5, operating the centrifugal system
Starting a conveying pump of a concentration tank to centrifuge the filtered and concentrated aluminum hydroxide solution, wherein two centrifugal separation operations are adopted during centrifugation, one centrifugal operation is firstly carried out by adopting one centrifugal machine, and the solution after the one centrifugal operation is conveyed into a temporary storage tank for temporary storage; then adopting a secondary centrifugal machine to carry out secondary centrifugal operation, and conveying the solution subjected to the secondary centrifugal operation to a storage tank for storage; waste liquid generated by the first centrifugal operation and the second centrifugal operation is conveyed to a waste liquid tank for storage;
detecting the ion content in the temporary storage tank through a multiparameter ion online detection control system of the temporary storage tank, and regulating and controlling the centrifugal speed, the centrifugal time, the centrifugal times and the injection water adding proportion of a centrifugal machine according to the ion content requirement;
detecting the content of aluminum ions in the storage tank by a multi-parameter ion online detection control system of the storage tank, and regulating and controlling the centrifugal speed, the centrifugal time, the centrifugal times and the injection water adding proportion of the two-channel centrifugal machine according to the content requirement of the aluminum ions;
step S6, operating the sterilization system
Conveying the aluminum hydroxide solution in the storage tank to a heat exchanger, heating, conveying to a sterilization tank, starting the sterilization tank for stirring, and performing damp-heat sterilization in the sterilization tank;
Step S7, operating the split charging system
And (5) conveying the aluminum hydroxide solution after the sterilization is qualified to an aseptic filling system, and starting to split into containers.
3. The process for producing aluminum hydroxide adjuvant based on an on-line inspection and control system according to claim 2, wherein in step S5, the centrifugal speed of the centrifuge is 3000-6000rpm, the centrifugal time is 30-50min, and the centrifugation is 2-5 times; the stirring time of the temporary storage tank is 10-30min, the stirring frequency is 300-500rpm, and the temporary storage tank circulates for 1-3 times; the centrifugal speed of the secondary centrifugal machine is 3000-6000rpm, the centrifugal time is 30-50min, and the centrifugal is carried out for 2-5 times; the stirring time of the storage tank is 30-60min, the stirring frequency is 300-500rpm, and the temperature is 60+/-2 ℃.
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