CN208500805U - A kind of reaction unit of solid phase method production acetylacetonate - Google Patents
A kind of reaction unit of solid phase method production acetylacetonate Download PDFInfo
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- CN208500805U CN208500805U CN201821009802.9U CN201821009802U CN208500805U CN 208500805 U CN208500805 U CN 208500805U CN 201821009802 U CN201821009802 U CN 201821009802U CN 208500805 U CN208500805 U CN 208500805U
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- reaction vessel
- reaction
- pentanedione
- acetylacetone
- main shaft
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Abstract
The utility model discloses a kind of reaction units of solid phase method production acetylacetonate, it include: motor and main shaft, the main shaft and shaft joint mechanical connection, the main shaft passes through the side wall of reaction vessel, it is sealed between the main shaft and the reaction vessel by seal box, the main shaft connects agitating paddle, temperature-measuring port in kettle is provided at the top of the reaction vessel, feeding inlet is provided at the top of the reaction vessel, the reaction container bottom is provided with discharge port, collet is provided on the reaction vessel outer wall, acetylacetone,2,4-pentanedione feed pot is provided with above the reaction vessel, condensation reflux device is provided with above the reaction vessel, nitrogen charging device a is provided with above the acetylacetone,2,4-pentanedione feed pot, micropore spray device is arranged in acetylacetone,2,4-pentanedione feed pot lower part, it solves prior-art devices acetylacetone,2,4-pentanedione and is easy leakage, produce acetyl Easily there is the problem of local excessive reaction, temperature increases and makes slow product discoloration, reaction, environmental pollution and feed blocking in acetone salt.
Description
Technical field
The utility model patent is related to producing the reaction unit of acetylacetonate, is a kind of solid phase method production specifically
The reaction unit of acetylacetonate.
Background technique
Solid phase method is the acetylacetonate new method for producing studied in recent years, and traditional liquid phase method needs a large amount of water to make
It is 10-15 times of acetylacetone,2,4-pentanedione additive amount for reaction medium, a large amount of waste water can be generated, and there is energy consumption height, low efficiency is dirty
Dye weight, the low disadvantage of production capacity.
Acetylacetone,2,4-pentanedione is a kind of toxic, corrosive liquid, and overflow will affect human health and ring during the reaction
The protection in border, the horizontal reactor that solid phase method uses have that poorly sealed or connector loosens in process of production, are easy
The problem of leakage, in addition easily there is local excessive reaction in prior art production acetylacetonate, and temperature increases and product is made to change colour
And the problem of feed blocking, the acetylacetonate first generated in reaction process can wrap unreacted material, will lead to anti-
It slowly should even react incomplete.
Utility model content
The utility model patent technical problems to be solved are: providing a kind of reaction dress of solid phase method production acetylacetonate
It sets, generates a large amount of waste water, energy consumption height to solve liquid phase method production acetylacetonate, low efficiency, pollution is heavy, the low disadvantage of production capacity,
Leakage is easy to solve prior-art devices acetylacetone,2,4-pentanedione, local excessive reaction easily occurs in production acetylacetonate, temperature raising
And the problem of making product discoloration, reaction slowly and feed blocking.
In order to achieve the above objectives, the technical solution of the utility model patent is: a kind of solid phase method production acetylacetonate
Reaction unit, comprising: motor, the motor and retarder mechanical connection, the retarder and shaft joint mechanical connection further include
Main shaft, the main shaft and shaft joint mechanical connection, the main shaft pass through the side wall of reaction vessel, the main shaft and described anti-
It answers and is sealed between container by seal box, the main shaft connects agitating paddle, it is provided with temperature-measuring port in kettle at the top of the reaction vessel,
It is provided with feeding inlet at the top of the reaction vessel, the reaction container bottom is provided with discharge port, on the reaction vessel outer wall
It is provided with collet, acetylacetone,2,4-pentanedione feed pot is provided with above the reaction vessel, is provided with and is condensed back to above the reaction vessel
Device is flowed, nitrogen charging device a is provided with above the acetylacetone,2,4-pentanedione feed pot, acetylacetone,2,4-pentanedione feed pot lower part is arranged micropore and sprays
Shower device.
Lower section is provided with steam (vapor) outlet and cooling water inlet, the folder of the reaction vessel on the left of the collet of the reaction vessel
Set right side top is provided with steam inlet and cooling water outlet.
Nitrogen charging device b is arranged in the discharge port side.
The agitating paddle is ∑ type high shear differential agitating paddle, frequency control.
The reaction vessel side wall, which is provided with, vacuumizes gas vent, described to vacuumize the external vacuum means of gas vent
It sets.
The reaction vessel, acetylacetone,2,4-pentanedione feed pot, micropore spray device and condensation reflux device material are titanium.
The seal box includes sealing box main body, abuts side wall on the left of reaction vessel, fastening nut on the right side of sealing box main body
Seal with screwed joint box main body and seal box gland, rubber air spring are socketed on fastening nut, the rubber of rubber air spring
It is provided with automatic inflatable device on glue air bag, is provided with airtight and watertight padding between seal box gland and reaction vessel.
The airtight and watertight padding is tetrafluoro packing.
The ratio of acetylacetone,2,4-pentanedione, the compound of metal and water with mass ratio for 38-44%:12-24%:38-44% is that starting is former
The compound of metal and water, are first added in the reaction vessel from feeding inlet, acetylacetone,2,4-pentanedione are then passed through levulinic by material
For the nitrogen charging device a and micropore spray device pressurized spray of ketone feed pot into the reaction vessel, shear agitation reacts 1.5-2
Hour, at negative pressure 0-0.1MPa, 30-80 DEG C of temperature, vacuum drying to get arrive acetylacetonate.
The compound of the metal is the change of the compound of calcium, the compound of zinc, the compound of magnesium, the compound of aluminium, iron
Close object, the compound of sodium, the compound of potassium or compound of lithium etc..
From the above technical scheme, the utility model has the advantages that:
1, it is sealed between the utility model main shaft and reaction vessel by seal box, seal box is tight by rubber air spring
Gu system compress airtight and watertight padding, solve each connector in main shaft continuous rotation easily loosens and airtight and watertight padding thermally expand cause slurry
The problem of solution is revealed, in addition, airtight and watertight padding uses tetrafluoro packing, tetrafluoro packing anticorrosive anti-wear, sealing effect is good, rubber air
Spring avoids that practical directly exposed spring is corroded or foreign matter falls into spring influences the elasticity of spring；
2, the utility model passes through the nitrogen charging device a and micropore spray device of acetylacetone,2,4-pentanedione feed pot, can make acetyl
Controllably uniformly reaction vessel is added in sprinkling to acetone from micropore spray device, and acetylacetone,2,4-pentanedione is contacted with the compound of metal, into
Row uniformly adequately reacts, while agitating paddle is ∑ type high shear differential agitating paddle, and frequency control keeps reaction more sufficiently and equal
It is even；
3, it is provided with condensation reflux device at the top of the utility model reaction vessel, the steam containing reactant is condensed and flowed back
Into reaction vessel, the waste of reaction raw materials is avoided, also avoids the pollution that steam is directly discharged in atmosphere；
4, nitrogen charging device b is arranged in the utility model discharge port side, and material during the reaction, intermittently will using nitrogen
The material remained in discharging port recess, which extrudes, participates in reaction, keeps reaction more complete, in addition, in blanking process, inflated with nitrogen
It can prevent feed blocking；
5, reaction vessel side wall described in the utility model, which is provided with, vacuumizes gas vent, vacuumizes gas vent connection and takes out
Vacuum plant, after the reaction was completed, product are not necessarily to filtration washing, vacuum drying are directly carried out in the reaction vessel, as catalysis
A small amount of water of agent is dry by heating, vacuum, environmental protection treatment is discharged in a manner of vapor, while making in the stirring of high shear force
Under, material is tentatively refined into coarse powder, crushes and screens finally by pulverizer, can be obtained finished product, and yield is close to theoretical value, matter
It measures reliable and stable.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of utility model device；
Fig. 2 is the enlarged diagram of utility model device seal box；
In figure: 1, acetylacetone,2,4-pentanedione feed pot, 2, nitrogen charging device a, 3, temperature-measuring port in kettle, 4, main shaft, 5, seal box, 6, anti-
Answer container, 7, agitating paddle, 8, collet, 9, feeding inlet, 10, condensation reflux device, 11, vacuumize gas vent, 12, steam inlet and
Cooling water outlet, 13, micropore spray device, 14, steam (vapor) outlet and cooling water inlet, 15, discharge port, 16, nitrogen charging device b,
5-1, sealing box main body, 5-2, seal box gland, 5-3, fastening nut, 5-4, rubber air spring, 5-5, automatic inflatable
Device.
Specific embodiment
1-2 further illustrates the utility model patent with reference to the accompanying drawing, it should be understood that the example is merely to illustrate practical
Novel rather than limitation the scope of the utility model, after having read the utility model, those skilled in the art are to this reality
The application range as defined in the appended claims is fallen with the modification of novel various equivalent forms.
The reaction unit of embodiment 1-3 is identical, sees following implementation:
A kind of reaction unit of solid phase method production acetylacetonate, comprising: motor, the motor and retarder machinery connect
It connects, the retarder and shaft joint mechanical connection, further include main shaft 4, the main shaft 4 and shaft joint mechanical connection, described
Main shaft 4 passes through the side wall of reaction vessel 6, is sealed between the main shaft 4 and the reaction vessel 6 by seal box 5, the main shaft
4 connect agitating paddles 7, are provided with temperature-measuring port 3 in kettle at the top of the reaction vessel 6, are provided with feeding inlet at the top of the reaction vessel 6
9,6 bottom of reaction vessel is provided with discharge port 15, is provided with collet 8, the reaction vessel on 6 outer wall of reaction vessel
6 tops are provided with acetylacetone,2,4-pentanedione feed pot 1, condensation reflux device 10 are provided with above the reaction vessel 6, the acetylacetone,2,4-pentanedione adds
Nitrogen charging device a2 is provided with above batch can 1, micropore spray device 13 is arranged in 1 lower part of acetylacetone,2,4-pentanedione feed pot.
The compound of acetylacetone,2,4-pentanedione and metal generates complex reaction under the catalysis of a small amount of water, and acetylacetone,2,4-pentanedione is added in when reaction
Liquid is too fast, will lead to the reaction of material local excessive, and temperature raising makes product change colour, influences product final mass, pass through acetyl
The nitrogen charging device a2 and micropore spray device 13 of acetone feed pot 1 can make acetylacetone,2,4-pentanedione controllably uniformly from micropore spray
Reaction vessel 6 is added in sprinkling in device 13, contacts with the compound of metal, carries out uniformly adequately reaction.
The acetylacetone,2,4-pentanedione condensing recovery of reaction volatilization is participated in reaction by condensation reflux device 10, keeps reaction more complete, simultaneously
Protect environment.
Temperature-measuring port 3 conveniently measures reaction temperature in kettle.
The 8 left side lower section of collet of the reaction vessel 6 is provided with steam (vapor) outlet and cooling water inlet 14, the reaction vessel
68 right side top of collet is provided with steam inlet and cooling water outlet 12, heats up and be passed through cooling water as desired by steam
It cools.
Nitrogen charging device b16 is arranged in 15 side of discharge port, and material during the reaction, will intermittently be remained using nitrogen
Material in 15 groove of discharge port, which extrudes, participates in reaction, keeps reaction more complete, in blanking process, inflated with nitrogen can prevent object
Material blocking.
The agitating paddle 7 is ∑ type high shear differential agitating paddle, frequency control.The acetylacetone,2,4-pentanedione first generated in reaction process
Salt can wrap unreacted material, will lead to reaction and slowly even react not exclusively, agitating paddle 7 stirs material in differential
It mixes and is come into full contact under the shear action of device offer, shear, react.
6 side wall of reaction vessel, which is provided with, vacuumizes gas vent 11, described to vacuumize the external pumping of gas vent 11 very
Empty device.After the reaction was completed, product is not necessarily to filtration washing, vacuum drying is directly carried out in reaction vessel 6, as catalyst
A small amount of water it is dry by heating, vacuum, environmental protection treatment is discharged in a manner of vapor, while in the stirring action of high shear force
Under, material is tentatively refined into coarse powder, crushes and screens finally by pulverizer, can be obtained finished product, and yield is close to theoretical value, quality
It is reliable and stable.
The reaction vessel 6, acetylacetone,2,4-pentanedione feed pot 1, micropore spray device 13 and 10 material of condensation reflux device are titanium,
With strong corrosion resistance.
The seal box 5 includes sealing box main body 5-1, abuts 6 left side side wall of reaction vessel on the right side of sealing box main body 5-1,
Fastening nut 5-3 seal with screwed joint box main body 5-1 and seal box gland 5-2, rubber air spring 5-4 are socketed in fastening nut
On 5-3, it is provided with automatic inflatable device 5-5 on the rubber pneumatic bag of rubber air spring 5-4, seal box gland 5-2 and anti-
It answers and is provided with airtight and watertight padding 5-6 between container 6, the airtight and watertight padding 5-6 is tetrafluoro packing, and tetrafluoro packing_seal effect is good, adopts
With inflated rubber spring 5-4 fastening system, the gland fastening nut 5-3 on stuffing box 5 is automatically adjusted, it is made to be in fastening forever
State enhances the reliability of sealing, overcomes the problems, such as that pulp solution is easy leakage in horizontal reactor.
The reactant ratio and technological parameter of embodiment 1-3 is as follows:
The compound of metal and water are added in the reaction vessel 6 from feeding inlet 9 first, agitating paddle 7 is opened, to metal
Compound and water be sufficiently mixed into scattered paste shape, close feeding inlet 9.Open steam inlet and cooling water outlet 12 and steam inlet
It is passed through cooling water with cooling water inlet 14, condenser device 10 opens 1 valve of acetylacetone,2,4-pentanedione feed pot, opens nitrogen charging device
A2, acetylacetone,2,4-pentanedione is sprayed from micropore spray device 13 is added reaction vessel 6, and sprinkling feed time control was at 15 minutes.Material exists
After abundant shear agitation is reacted 2 hours in reaction vessel 6, it is vented cooling water, open steam inlet and cooling water outlet 12 and is steamed
Vapor inlet and cooling water inlet 14 are passed through cooling water and are passed through steam, the vacuum evacuation device for vacuumizing gas vent 11 are opened, in reality
The negative pressure of example is applied persistently stirring drying 2 hours at a temperature of.Vapor is discharged from gas vent 11 is vacuumized, end to be dried
Afterwards, each valve is closed.Reacting drying terminates to obtain coarse powder, is crushed by pulverizer and obtains acetylacetonate finished product.Embodiment 1
Obtained calcium acetylacetonate (in terms of dry product) finished product net yield is 98.5%, and the zinc acetylacetonate that embodiment 2 obtains is (with dry product
Meter) finished product net yield be 98.2%, magnesium acetylacetonate (in terms of dry product) the finished product net yield that embodiment 3 obtains be 98.0%.
The above is only the preferred embodiment of the utility model, it is noted that for the common skill of the art
For art personnel, without departing from the principle of this utility model, several improvements and modifications can also be made, these improve and
Retouching also should be regarded as the protection scope of the utility model.
Claims (8)
1. a kind of reaction unit of solid phase method production acetylacetonate, comprising: motor, the motor and retarder mechanical connection,
The retarder and shaft joint mechanical connection, it is characterised in that: it further include main shaft (4), the main shaft (4) and the shaft joint machine
Tool connection, the main shaft (4) pass through the side wall of reaction vessel (6), pass through between the main shaft (4) and the reaction vessel (6)
Seal box (5) sealing, the main shaft (4) connect agitating paddle (7), are provided with temperature-measuring port in kettle at the top of the reaction vessel (6)
(3), it is provided with feeding inlet (9) at the top of the reaction vessel (6), reaction vessel (6) bottom is provided with discharge port (15), institute
It states and is provided with collet (8) on reaction vessel (6) outer wall, be provided with acetylacetone,2,4-pentanedione feed pot (1) above the reaction vessel (6),
It is provided with condensation reflux device (10) above the reaction vessel (6), is provided with inflated with nitrogen above the acetylacetone,2,4-pentanedione feed pot (1)
Device a(2), micropore spray device (13) are arranged in acetylacetone,2,4-pentanedione feed pot (1) lower part.
2. a kind of reaction unit of solid phase method production acetylacetonate according to claim 1, which is characterized in that described anti-
Lower section on the left of the collet (8) of container (6) is answered to be provided with steam (vapor) outlet and cooling water inlet (14), the folder of the reaction vessel (6)
Top is provided with steam inlet and cooling water outlet (12) on the right side of set (8).
3. a kind of reaction unit of solid phase method production acetylacetonate according to claim 1, which is characterized in that it is described go out
Nitrogen charging device b(16 is arranged in material mouth (15) side).
4. a kind of reaction unit of solid phase method production acetylacetonate according to claim 1, which is characterized in that described to stir
Mixing paddle (7) is ∑ type high shear differential agitating paddle, frequency control.
5. a kind of reaction unit of solid phase method production acetylacetonate according to claim 1, which is characterized in that described anti-
It answers container (6) side wall to be provided with to vacuumize gas vent (11), it is described to vacuumize gas vent (11) external vacuum evacuation device.
6. a kind of reaction unit of solid phase method production acetylacetonate according to claim 1, which is characterized in that described anti-
Answering container (6), acetylacetone,2,4-pentanedione feed pot (1), micropore spray device (13) and condensation reflux device (10) material is titanium.
7. a kind of reaction unit of solid phase method production acetylacetonate according to claim 1, which is characterized in that described close
Joint sealing (5) includes sealing box main body (5-1), abuts side wall on the left of reaction vessel (6) on the right side of sealing box main body (5-1), fastens spiral shell
Female (5-3) seal with screwed joint box main body (5-1) and seal box gland (5-2), rubber air spring (5-4) are socketed in fastening spiral shell
On female (5-3), automatic inflatable device (5-5), seal box gland are provided on the rubber pneumatic bag of rubber air spring (5-4)
Airtight and watertight padding (5-6) is provided between (5-2) and reaction vessel (6).
8. a kind of reaction unit of solid phase method production acetylacetonate according to claim 7, which is characterized in that described close
Packing material (5-6) is tetrafluoro packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821009802.9U CN208500805U (en) | 2018-06-28 | 2018-06-28 | A kind of reaction unit of solid phase method production acetylacetonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821009802.9U CN208500805U (en) | 2018-06-28 | 2018-06-28 | A kind of reaction unit of solid phase method production acetylacetonate |
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| Publication Number | Publication Date |
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| CN208500805U true CN208500805U (en) | 2019-02-15 |
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| CN201821009802.9U Active CN208500805U (en) | 2018-06-28 | 2018-06-28 | A kind of reaction unit of solid phase method production acetylacetonate |
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Denomination of utility model: A reaction device for producing acetylacetone salt by solid phase method Effective date of registration: 20210816 Granted publication date: 20190215 Pledgee: Bank of Huzhou Limited by Share Ltd. Pledgor: HUZHOU CITY LINGHU XINWANG CHEMICAL Co.,Ltd. Registration number: Y2021990000725 |