CN108355596A - A kind of proportioner and proportioning process taking heat drop low temperature using raw material - Google Patents

A kind of proportioner and proportioning process taking heat drop low temperature using raw material Download PDF

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Publication number
CN108355596A
CN108355596A CN201810169018.2A CN201810169018A CN108355596A CN 108355596 A CN108355596 A CN 108355596A CN 201810169018 A CN201810169018 A CN 201810169018A CN 108355596 A CN108355596 A CN 108355596A
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cooling
raw material
batching kettle
cool
coil pipe
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CN108355596B (en
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潘亚文
王振江
张鑫
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China Tianchen Engineering Corp
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China Tianchen Engineering Corp
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • 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
    • B01F35/90Heating or cooling systems
    • B01F35/91Heating or cooling systems using gas or liquid injected into the material, e.g. using liquefied carbon dioxide or steam
    • 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
    • B01F35/90Heating or cooling systems
    • B01F35/92Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00Catalysts comprising molecular sieves
    • B01J29/04Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/40Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/26Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
    • B01J31/38Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25DREFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D31/00Other cooling or freezing apparatus
    • 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
    • B01F35/90Heating or cooling systems
    • B01F2035/98Cooling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/2204Mixing chemical components in generals in order to improve chemical treatment or reactions, independently from the specific application
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094Jackets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00121Controlling the temperature by direct heating or cooling
    • B01J2219/00123Controlling the temperature by direct heating or cooling adding a temperature modifying medium to the reactants
    • B01J2219/00126Cryogenic coolants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/18Details relating to the spatial orientation of the reactor
    • B01J2219/185Details relating to the spatial orientation of the reactor vertical

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Accessories For Mixers (AREA)

Abstract

The present invention provides a kind of proportioner and proportioning process taking heat drop low temperature using raw material, device includes batching kettle and cooling & cool-storing apparatus;The heat production coil pipe being connected to by pipeline with cooling & cool-storing apparatus is equipped in the batching kettle, outside is equipped with the cooling jacket being connected to by pipeline with cooling & cool-storing apparatus;Cold-storage raw material is housed in the cooling & cool-storing apparatus;The heat production coil pipe is equipped in several through tubes and the hole outside pipe.Proportioner of the present invention effectively avoids the variation of local temperature in batching kettle to the influence of material reaction, and can reduce production cost with feed proportioning optimization technique simultaneously;Device of the present invention discharges big calorimetric suitable for blending process, and needs to maintain the temperature at a certain range of technique in blending process.

Description

A kind of proportioner and proportioning process taking heat drop low temperature using raw material
Technical field
The invention belongs to chemical equipment technical fields, take the dispensing of heat drop low temperature to fill using raw material more particularly, to a kind of It sets.
Background technology
In chemical industry, certain materials will present exothermic reaction in blending process, releases a large amount of heat, may can also Whole system is had an impact, unnecessary influence is generated on the novel substance being synthetically produced.Common heat sink is using cold But chuck cools down to reaction kettle, and cooling jacket is equipped with refrigerant, but since cooling jacket can only drop reaction kettle part Temperature can not achieve the complete cooling inside raw material, cause by-product more, it is therefore desirable to make every effort to keep dispensing in blending process The temperature of kettle stablizes the project for becoming and needing to study at present.
Invention content
In view of this, the present invention is directed to propose a kind of proportioner taking heat drop low temperature using raw material, existing to overcome The deficiency of technology effectively avoids the variation of local temperature in batching kettle to the influence of material reaction, and simultaneously can be with feed proportioning optimization Technique reduces production cost;Device of the present invention discharges big calorimetric suitable for blending process, and is needed in blending process Maintain the temperature at a certain range of technique.
In order to achieve the above objectives, the technical proposal of the invention is realized in this way:
A kind of proportioner taking the low autoclave body temperature of heat drop using raw material, including batching kettle and cooling & cool-storing apparatus;Institute The heat production coil pipe for being equipped in batching kettle and being connected to by pipeline with cooling & cool-storing apparatus is stated, outside is equipped with to be passed through with cooling & cool-storing apparatus The cooling jacket of pipeline connection;
Cold-storage raw material is housed in the cooling & cool-storing apparatus;The heat production coil pipe is equipped in several through tubes and outside pipe Hole.
Existing refrigerating plant may be used in cooling & cool-storing apparatus, realizes the cooling of its built-in cold-storage raw material, cold-storage Function only needs to can be realized the shell of device using attemperator.
Further, the discharge port of the cooling & cool-storing apparatus is connected with charging supervisor, and charging supervisor passes through the first branch pipe With the inlet communication of heat production coil pipe;Inlet communication of the supervisor by the second branch pipe and cooling jacket is fed simultaneously;
The refluxing opening of the cooling & cool-storing apparatus is connected with return main;Return main passes through third branch pipe and heat production coil pipe Refluxing opening connection;And return main is connected to by the 4th branch pipe with the refluxing opening of cooling jacket.
In order to reduce the cost of equipment, one return main of setting is then in place to be shunted, by cold-storage raw material point It is fitted in heat production coil pipe and cooling jacket.
Further, charging supervisor is equipped with circulating pump, the upper and lower stream of circulating pump be respectively equipped with the first valve and Second valve;First branch pipe is equipped with third valve;Third branch pipe is equipped with the 5th valve;4th branch pipe is equipped with the 4th valve Door.The disengaging cold-storage raw material of heat production coil pipe and cooling jacket can be controlled respectively, according to demand, it is determined whether open or close Valve closing door;Here each valve can be the adjustable existing valve of flow, to realize the interior of heat production coil pipe and cooling jacket The flow velocity of cold-storage raw material it is adjustable, to realize the adjustable of dispensing temperature in the kettle.
Further, the position of the upper discharge port close to cooling & cool-storing apparatus of charging supervisor is equipped with discharge valve;Reflux master On pipe return valve is equipped with close to the position of the refluxing opening of cooling & cool-storing apparatus.
Further, agitating paddle is equipped in the batching kettle, and the top of batching kettle is equipped with the electricity for driving agitating paddle rotation Machine.
Further, cold-storage raw material is one kind in water, ethylene glycol, acid solution, metal salt solution, aqueous slkali, benzene, chlorobenzene Or it is several.
Further, the import of the heat production coil pipe and refluxing opening are respectively positioned on the top of batching kettle, and heat production coil pipe Bottom end is located between the bottom end and the bottom end of agitating paddle of batching kettle, and heat production coil pipe is arranged in batching kettle arrives suitable position, It is uniform to be more conducive to injection of the cold-storage material in batching kettle, realizes uniform cooling;
The import of the cooling jacket is located at its lower end, and the refluxing opening of cooling jacket is at its upper end, and cooling jacket is under It holds into cold-storage raw material, then flows back from upper end, convenient for the cold-storage raw material thermal energy as much as possible for absorbing batching kettle, extend and absorb heat The time of energy.
Further, the heat production coil pipe the side towards agitating paddle be equipped with several through tubes in the circular hole outside pipe, And the distribution density of circular hole is gradually reduced from top to bottom on heat production coil pipe.Since the thermal energy that lower section generates is unfavorable for distributing, top Heat dissipation is very fast, therefore the circular hole density below heat production coil pipe is increased, and cold-storage raw material as much as possible is made to enter dispensing from below In kettle.
Further, further include temperature measuring equipment, the detecting head of temperature measuring equipment is located in batching kettle.Temperature measuring equipment can be with oneself Control system connects, and then also connect each valve with robot control system(RCS) simultaneously, realizes the automation control of entire proportioner.
Further, material total volume is the 30~70% of batching kettle volume in the batching kettle.
It is a kind of using proportioner as described above carry out dispensing technique, include the following steps, by ZSM-5 molecular sieve with Sodium hydroxide solution is added in batching kettle, the uniform stirring 2-8h at 40-80 DEG C, rotating speed of agitator 30-100r/min, then Cold-storage raw material in cooling & cool-storing apparatus is uniformly ejected into 10-30L/min in batching kettle 7 by heat production coil pipe, it is lasting to spray Time about 0.5-3h is penetrated, blender is stirred with 30-100r/min, when temperature is increased to 50-75 DEG C, opens cooling jacket Reinforcement cooling function is carried out, cooling jacket is then closed when temperature is less than 30-40 DEG C, continues that 3-8h is mixed;The cold-storage Raw material is the sulfuric acid solution or ammonium phosphate solution of 0.1-2.0mol/L;After cold-storage raw material in heat production coil pipe stops injection, match The mass ratio of ZSM-5 molecular sieve, NaOH and the sulfuric acid or phosphoric acid that are added in material kettle is 1:(0.05-1):(0.1-1).
A kind of technique being carried out dispensing using proportioner as described above, is included the following steps, is 5- by mass fraction 25% tetrapropylammonium hydroxide solution is put into batching kettle, rotating speed of agitator 50-300r/min, by organic amine mixed liquor It is added in batching kettle with the speed of 10-50mL/min, then proceedes to stirring 3-6h, then by organic silicon source and fatty alcohol, organic Titanium source is added with the speed of 10-50mL/min in batching kettle respectively, then by the aliphatic acid in cooling & cool-storing apparatus by taking heat Coil pipe is ejected into the speed of 1-5mL/min in batching kettle, ensures that the temperature in batching kettle is maintained at 20-40 DEG C when addition, after Continuous stirring 1-5h opens cooling jacket and carries out reinforcement cooling function when temperature is increased to 35~45 DEG C, when temperature less than 18~ Cooling jacket is then closed at 24 DEG C;After cold-storage raw material in heat production coil pipe stops injection, the tetrapropyl hydrogen of addition in batching kettle (7) Amine-oxides, organic amine, organic silicon source, fatty alcohol, organic titanium source, aliphatic acid mass ratio be (2-20):(0.02-2):(10- 20):(20-50):1:(0.05-1).
Compared with the existing technology, the proportioner of the present invention that heat drop low temperature is taken using raw material is had following excellent Gesture:
(1) proportioner of the present invention overcomes heat exchange single in the prior art, excessively time consumption and energy consumption, And influence the defect of manufacturing schedule;The present invention is equipped with heat production coil pipe and cooling jacket simultaneously, and heat production coil pipe can be by cooling Raw material be added in batching kettle, when the material quantity of addition has reached requirement, exothermic process has been completed substantially, The cooling of cooling jacket is only needed to can guarantee the demand of cooling.
(2) proportioner of the present invention, cool storage medium are one of the raw material in blending process, and in batching kettle Heat production coil pipe is equipped with some ducts, and when needing dispensing, batching kettle is sprayed onto by being pressurized from duct as the raw material of cool storage medium In, it is mixed with slurries, since the raw material sprayed from duct is cooling, the temperature of slurries whole interior can be reduced, it is quickly real The reduction of existing dispensing temperature in the kettle, and avoid the only reduction of local temperature in batching kettle.
(3) proportioner of the present invention can be relatively low in nocturnal temperature and to use due to the use of cooling & cool-storing apparatus When electric peak valley, refrigeration operation is carried out, then cooling cold-storage raw material is stored in cool storage medium, when carrying out dispensing, is passed through Cold-storage raw material takes cold energy to batching kettle, realizes the uniform decrease in temperature in batching kettle, is shifted on the time for realizing using energy source Simultaneously, it is ensured that without the generation of excessive industrial wastes.
(4) temperature measuring equipment is set, the temperature in batching kettle is monitored, by adjusting the matching relationship of each valve, is adjusted The flow velocity for saving cold-storage raw material achievees the purpose that adjust the temperature in batching kettle, operation letter to accelerate or slow down heat exchanging process Single, controllability is strong.
Description of the drawings
The attached drawing for constituting the part of the present invention is used to provide further understanding of the present invention, schematic reality of the invention Example and its explanation are applied for explaining the present invention, is not constituted improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is a kind of to take the simple structure of the proportioner of heat drop low temperature to show using raw material described in the embodiment of the present invention It is intended to;
Reference sign:
1, cooling & cool-storing apparatus;2, cold-storage raw material;3, circulating pump;4, agitating paddle;5, cooling jacket;6, heat production coil pipe;7、 Batching kettle;8, motor;9, temperature measuring equipment;10, charging supervisor;11, the first branch pipe;12, the second branch pipe;13, third branch pipe;14、 4th branch pipe;15, return main;16, discharge valve;17, the first valve;18, the second valve;19, third valve;20, the 4th Valve;21, the 5th valve;22, return valve.
Specific implementation mode
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase Mutually combination.
In the description of the present invention, it is to be understood that, term "center", " longitudinal direction ", " transverse direction ", "upper", "lower", The orientation or positional relationship of the instructions such as "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside" is It is based on the orientation or positional relationship shown in the drawings, is merely for convenience of description of the present invention and simplification of the description, rather than instruction or dark Show that signified device or element must have a particular orientation, with specific azimuth configuration and operation, therefore should not be understood as pair The limitation of the present invention.In addition, term " first ", " second " etc. are used for description purposes only, it is not understood to indicate or imply phase To importance or implicitly indicate the quantity of indicated technical characteristic.The feature for defining " first ", " second " etc. as a result, can To express or implicitly include one or more this feature.In the description of the present invention, unless otherwise indicated, " multiple " It is meant that two or more.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected;It can Can also be electrical connection to be mechanical connection;It can be directly connected, can also indirectly connected through an intermediary, Ke Yishi Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood by concrete condition Concrete meaning in the present invention.
The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
As shown in Figure 1, a kind of proportioner taking heat drop low temperature using raw material, including batching kettle 7 and refrigeration and cold accumulation Device 1;The heat production coil pipe 6 being connected to by pipeline with cooling & cool-storing apparatus 1 is equipped in the batching kettle 7, outside is equipped with and refrigeration The cooling jacket 5 that cold-storage device 1 is connected to by pipeline;
Cold-storage raw material 2 is housed in the cooling & cool-storing apparatus 1;The heat production coil pipe 6 is equipped in several through tubes and pipe Outer hole.
The discharge port of the cooling & cool-storing apparatus 1 is connected with charging supervisor 10, charging supervisor 10 by the first branch pipe 11 with The inlet communication of heat production coil pipe 6;Inlet communication of the supervisor 10 by the second branch pipe 12 and cooling jacket 5 is fed simultaneously;
The refluxing opening of the cooling & cool-storing apparatus 1 is connected with return main 15;Return main 15 by third branch pipe 13 with The refluxing opening of heat production coil pipe 6 is connected to;And return main 15 is connected to by the 4th branch pipe 14 with the refluxing opening of cooling jacket 5.
Charging supervisor 10 is equipped with circulating pump 3, and the upper and lower stream of circulating pump 3 is respectively equipped with the first valve 17 and the Two valves 18;First branch pipe 11 is equipped with third valve 19;Third branch pipe 13 is equipped with the 5th valve 21;It is set on 4th branch pipe 14 There is the 4th valve 20.
The position of discharge port on charging supervisor 10 close to cooling & cool-storing apparatus 1 is equipped with discharge valve 16;Return main 15 The position of the upper refluxing opening close to cooling & cool-storing apparatus 1 is equipped with return valve 22.
Agitating paddle 4 is equipped in the batching kettle 7, and the top of batching kettle 7 is equipped with the motor 8 for driving agitating paddle 4 to rotate.
Cold-storage raw material 2 is one or more of water, ethylene glycol, acid solution, metal salt solution, aqueous slkali, benzene, chlorobenzene.
The import of the heat production coil pipe 6 and refluxing opening are respectively positioned on the top of batching kettle 7, and the bottom end position of heat production coil pipe 6 Between the bottom end of batching kettle 7 and the bottom end of agitating paddle 4;
The import of the cooling jacket 5 is located at its lower end, and the refluxing opening of cooling jacket 5 is at its upper end.
The heat production coil pipe 6 is equipped in several through tubes in the side towards agitating paddle 4 with the circular hole outside pipe, and takes hot plate The distribution density of circular hole is gradually reduced from top to bottom on pipe 6.
Further include temperature measuring equipment 9, the detecting head of temperature measuring equipment 9 is located in batching kettle 7.
Material total volume is the 30~70% of 7 volume of batching kettle in the batching kettle 7.
The course of work:
Cold-storage raw material 2 is freezed in cooling & cool-storing apparatus 1, and keeps temperature;When needing dispensing, by other originals Material is added in batching kettle 7, opens the motor 8 of agitating paddle 4, is then turned on discharge valve 16, the first valve 17, the second valve 18, third valve 19 and the 4th valve 20 realize that heat production coil pipe 6 sprays cold-storage raw material 2 in batching kettle, while realizing cooling The flowing of cold-storage raw material 2 in chuck 5;
When the cold-storage raw material 2 being added in batching kettle 7 has reached the amount needed for reaction, 11 are closed;At this time due to Exothermic process is over, it is only necessary to the effect of cooling jacket 5;
When adjusting third valve 19 and the 5th valve 21, realize the flow velocity in heat production coil pipe 6, and can according to 21 switch Size realizes the pressure adjustable in heat production coil pipe 6.
When adjusting four valves 20, the adjustable of the cold-storage residence time of raw material in cooling jacket 5 is realized.
The cold-storage raw material 2 of reflux is flowed back by return main 15 in cooling & cool-storing apparatus 1, is according to actual demand decision It is no during the work time, open refrigerating function;
A surge tank can also be added on return main 15, temporarily deposit is delaying by the cold-storage raw material 2 after absorption heat It rushes in tank, prevents the cold-storage raw material 2 after absorption heat from being mixed with the cold-storage raw material 2 in cooling & cool-storing apparatus 1;To the end of reaction Afterwards, the cold-storage raw material 2 after the natural cooling in surge tank is imported in cooling & cool-storing apparatus 1;
After the completion of a work period, raw material is supplemented in cooling & cool-storing apparatus 1 as needed.
Experimental example 1
Cyclohexene hydration catalyst:ZSM-5 molecular sieve and sodium hydroxide solution are added in batching kettle 7, stirred at 60 DEG C It is 80r/min uniform stirring 4h to mix device rotating speed, then by the sulfuric acid solution of the cold-storage raw material 1mol/L in cooling & cool-storing apparatus 1 or Person's ammonium phosphate solution is uniformly ejected into 20L/min in batching kettle 7 by heat production coil pipe 6, sustained firing time about 2h, blender It is stirred with 65r/min, when temperature is increased to 65 DEG C, opens cooling jacket and carry out reinforcement cooling function, when temperature is less than Cooling jacket is then closed at 35 DEG C, continues that 6h is mixed, this is in the process it is also ensured that make cooling in the case of proper temperature The flowing of cold-storage raw material in chuck 5.Using this method prepare catalyst granules it is more uniform, reduce smaller particle and compared with The quantity of the substandard product of bulky grain.The particle uniformity coefficient of catalyst is set to improve 5-15%;
After stopping injection, the mass ratio of ZSM-5 molecular sieve, NaOH and the sulfuric acid or phosphoric acid that are added in batching kettle 7 is 1: 0.07:0.6.Organic amine is n-butylamine, organic silicon source is silester, fatty alcohol is isopropanol, organic titanium source is four fourth of metatitanic acid Ester.
Embodiment 2
Oximes catalyst:The tetrapropylammonium hydroxide solution that mass fraction is 15% is put into batching kettle, rotating speed Under being stirred for 150r/min, organic amine mixed liquor is added with the speed of 20mL/min in batching kettle, then proceedes to stirring 4h, so Organic silicon source and fatty alcohol, organic titanium source are added with the speed of 35mL/min in batching kettle respectively afterwards, agitator speed is 200r/min is stirred evenly, and then the aliphatic acid in cooling & cool-storing apparatus is added in batching kettle with the speed of 4mL/min, is added When ensure batching kettle in temperature be maintained at 30 DEG C, continue stir 3h, when temperature is increased to 40, open cooling jacket added Strong cooling function then closes cooling jacket 5 when temperature is less than 20 DEG C, continues to be mixed, this is in the process it is also ensured that temperature Degree makes the flowing of the cold-storage raw material in cooling jacket 5 suitable in the case of.After cold-storage raw material 2 in heat production coil pipe 6 stops injection, The mass ratio of the tetrapropylammonium hydroxide, organic amine, organic silicon source, fatty alcohol, organic titanium source, aliphatic acid that are added in batching kettle 7 It is 5:0.5:17:40:1:0.2.Organic amine is n-butylamine, organic silicon source is silester, fatty alcohol is isopropanol, organic titanium source For butyl titanate.
The catalyst granules prepared using this method is more uniform, reduces the unqualified production of smaller particle and larger particles The quantity of product.The particle uniformity coefficient of catalyst is set to improve 10%-20%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.

Claims (10)

1. a kind of proportioner taking heat drop low temperature using raw material, it is characterised in that:Including batching kettle (7) and refrigeration and cold accumulation Device (1);The heat production coil pipe (6) being connected to by pipeline with cooling & cool-storing apparatus (1) is equipped in the batching kettle (7), outside is set There is the cooling jacket (5) being connected to by pipeline with cooling & cool-storing apparatus (1);
Cold-storage raw material (2) is housed in the cooling & cool-storing apparatus (1);The heat production coil pipe (6) be equipped with several through tubes in Hole outside pipe.
2. the proportioner according to claim 1 for taking heat drop low temperature using raw material, it is characterised in that:The refrigeration stores The discharge port of device for cooling (1) is connected with charging supervisor (10), and charging supervisor (10) passes through the first branch pipe (11) and heat production coil pipe (6) Inlet communication;Feed inlet communication of the supervisor (10) by the second branch pipe (12) and cooling jacket (5) simultaneously;
The refluxing opening of the cooling & cool-storing apparatus (1) is connected with return main (15);Return main (15) passes through third branch pipe (13) it is connected to the refluxing opening of heat production coil pipe (6);And return main (15) passes through time of the 4th branch pipe (14) and cooling jacket (5) Head piece is connected to.
3. the proportioner according to claim 2 for taking heat drop low temperature using raw material, it is characterised in that:The charging master It manages (10) and is equipped with circulating pump (3), the upper and lower stream of circulating pump (3) is respectively equipped with the first valve (17) and the second valve (18); First branch pipe (11) is equipped with third valve (19);Third branch pipe (13) is equipped with the 5th valve (21);On 4th branch pipe (14) Equipped with the 4th valve (20);Preferably, it is equipped with out close to the position of the discharge port of cooling & cool-storing apparatus (1) on charging supervisor (10) Expect valve (16);On return main (15) return valve (22) is equipped with close to the position of the refluxing opening of cooling & cool-storing apparatus (1).
4. the proportioner according to claim 1 for taking heat drop low temperature using raw material, it is characterised in that:The batching kettle (7) agitating paddle (4) is equipped in, and the top of batching kettle (7) is equipped with the motor (8) for driving agitating paddle (4) to rotate;
Preferably, the import of the heat production coil pipe (6) and refluxing opening are respectively positioned on the top of batching kettle (7), and heat production coil pipe (6) Bottom end be located between the bottom end of batching kettle (7) and the bottom end of agitating paddle (4);
The import of the cooling jacket (5) is located at its lower end, and the refluxing opening of cooling jacket (5) is at its upper end.
5. the proportioner according to claim 1 for taking heat drop low temperature using raw material, it is characterised in that:Cold-storage raw material (2) it is one or more of water, ethylene glycol, acid solution, metal salt solution, aqueous slkali, benzene, chlorobenzene, aliphatic acid.
6. the proportioner according to claim 1 for taking heat drop low temperature using raw material, it is characterised in that:It is described to take hot plate Manage (6) the side towards agitating paddle (4) be equipped with several through tubes in pipe outside circular hole, and on heat production coil pipe (6) from it is lower to The distribution density of upper circular hole is gradually reduced.
7. the proportioner according to claim 1 for taking heat drop low temperature using raw material, it is characterised in that:It further include thermometric The detecting head of device (9), temperature measuring equipment (9) is located in batching kettle (7).
8. the proportioner according to claim 1 for taking heat drop low temperature using raw material, it is characterised in that:The batching kettle (7) material total volume is the 30~70% of batching kettle (7) volume in.
9. a kind of technique carrying out dispensing using such as claim 1~8 any one of them proportioner, it is characterised in that:Packet Following steps are included, ZSM-5 molecular sieve and 0.1-3mol/L sodium hydroxide solutions are added in batching kettle (7), at 40-80 DEG C Even stirring 2-8h, agitating paddle (4) rotating speed are 30-100r/min, then that the cold-storage raw material (2) in cooling & cool-storing apparatus (1) is logical It crosses heat production coil pipe (6) to be uniformly ejected into batching kettle 7 with 10-30L/min, sustained firing time about 0.5-3h, blender is with 30- 100r/min is stirred, and when temperature is increased to 50-75 DEG C, is opened cooling jacket and is carried out reinforcement cooling function, when temperature is low Cooling jacket is then closed when 30-40 DEG C, continues that 3-8h is mixed;The cold-storage raw material (2) is the sulphur of 0.1-2.0mol/L Acid solution or ammonium phosphate solution;After cold-storage raw material (2) in heat production coil pipe (6) stops injection, it is added in batching kettle (7) The mass ratio of ZSM-5 molecular sieve, NaOH and sulfuric acid or ammonium phosphate is 1:(0.05-1):(0.1-1).
10. a kind of technique carrying out dispensing using such as claim 1~8 any one of them proportioner, it is characterised in that:Packet Following steps are included, the tetrapropylammonium hydroxide solution that mass fraction is 5-25% are put into batching kettle (7), agitating paddle (4) Rotating speed is 50-300r/min, and organic amine mixed liquor is added with the speed of 10-50mL/min in batching kettle (7), then proceedes to stir 3-6h is mixed, then organic silicon source and fatty alcohol, organic titanium source are added with the speed of 10-50mL/min in batching kettle (7) respectively, Then the aliphatic acid in cooling & cool-storing apparatus (1) is ejected into batching kettle by heat production coil pipe (6) with the speed of 1-5mL/min (7) ensure that the temperature in batching kettle (7) is maintained at 20-40 DEG C in, when addition, continue to stir 1-5h, when temperature is increased to 35~ At 45 DEG C, opens cooling jacket and carry out reinforcement cooling function, cooling jacket is then closed when temperature is less than 18~24 DEG C;Take hot plate It manages the cold-storage raw material (2) in (6) to stop after spraying, the tetrapropylammonium hydroxide of addition, organic amine, organosilicon in batching kettle (7) Source, fatty alcohol, organic titanium source, aliphatic acid mass ratio be (2-20):(0.02-2):(10-20):(20-50):1:(0.05- 1)。
CN201810169018.2A 2018-02-28 2018-02-28 Batching device and batching process for reducing temperature by using raw material heat extraction Active CN108355596B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110639459A (en) * 2019-10-10 2020-01-03 万华化学集团股份有限公司 Device and method for preparing 1-octene by ethylene selective oligomerization

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CN204234035U (en) * 2014-05-06 2015-04-01 山东金泽利能源科技有限公司 A kind of Gas Stirring still being easy to heat
CN204996452U (en) * 2015-09-16 2016-01-27 江西维莱营健高科有限公司 Health food makes and uses reaction kettle device
CN205146197U (en) * 2015-11-04 2016-04-13 玉门油田科达化学有限责任公司 Reation kettle heats outer circulative cooling system
CN105536675A (en) * 2015-12-28 2016-05-04 金爱莲 Reaction device
CN206881716U (en) * 2017-07-13 2018-01-16 黑龙江工业学院 Chemical reaction kettle

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Publication number Priority date Publication date Assignee Title
CN204234035U (en) * 2014-05-06 2015-04-01 山东金泽利能源科技有限公司 A kind of Gas Stirring still being easy to heat
CN204996452U (en) * 2015-09-16 2016-01-27 江西维莱营健高科有限公司 Health food makes and uses reaction kettle device
CN205146197U (en) * 2015-11-04 2016-04-13 玉门油田科达化学有限责任公司 Reation kettle heats outer circulative cooling system
CN105536675A (en) * 2015-12-28 2016-05-04 金爱莲 Reaction device
CN206881716U (en) * 2017-07-13 2018-01-16 黑龙江工业学院 Chemical reaction kettle

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110639459A (en) * 2019-10-10 2020-01-03 万华化学集团股份有限公司 Device and method for preparing 1-octene by ethylene selective oligomerization

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