CN107056597A - The technique and device of a kind of solid phase method production zinc acetylacetonate - Google Patents
The technique and device of a kind of solid phase method production zinc acetylacetonate Download PDFInfo
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- CN107056597A CN107056597A CN201710391053.4A CN201710391053A CN107056597A CN 107056597 A CN107056597 A CN 107056597A CN 201710391053 A CN201710391053 A CN 201710391053A CN 107056597 A CN107056597 A CN 107056597A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/77—Preparation of chelates of aldehydes or ketones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1856—Stationary reactors having moving elements inside placed in parallel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
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Abstract
The invention discloses the technique that a kind of solid phase method produces zinc acetylacetonate, it is characterised in that：Acetylacetone,2,4-pentanedione, the compound of zinc and water are using mass ratio as 38 42%:16‑24%:38 42% ratio is added in homemade high shear reaction unit, and shear agitation is reacted 1.5 2 hours, under the 0.1MPa of negative pressure 0,30 60 DEG C of temperature, vacuum drying, that is, obtains zinc acetylacetonate.
Description
Technical field
The present invention relates to a kind of technique and device for producing zinc acetylacetonate, more particularly to a kind of solid phase method production levulinic
The technique and device of ketone zinc.
Background technology
With polyvinyl chloride（PVC）All types of plastic product can be produced for primary raw material, including it is sheet material, tubing, pipe fitting, different
The soft goods such as the boardy products such as section bar material and film, pipe, footwear, toy, CABLE MATERIALS, artificial leather, should in terms of articles for daily use, industrial or agricultural
With extensive.However, because PVC material easily produces thermal degradation during processing and use, causing color burn, properties
Also decrease, it is therefore necessary to add stabilizer to prevent or alleviate its thermal degradation during processing and use.It is thermally-stabilised
Agent species is various, mainly including lead salts, metallic soap, organo-tin compound, organic stabilizer and the major class of compound stabilizer five.With
The successive appearance of the multinomial regulation such as European Union and China, both at home and abroad to the environmental requirement more and more higher of heat stabilizer, lead etc. is containing weight
The heat stabilizer of metal is gradually prohibited from using, and the development and application of nontoxic, environmentally friendly type thermal stabilizing agent turns into main development side
To.Beta-diketon class substance toxicity is low, can significantly improve PVC initial coloration performance, extend its heat-stable time, is a kind of level tool
The auxiliary heat stabilizer of development prospect.There is very strong complexing power yet with beta-diketon class material, easily make PVC rubescent,
Therefore, generally beta-diketon and zinc are complexed, its complexing power are reduced, so as to weaken its coloring to PVC product.Acetylacetone,2,4-pentanedione is just
Simplest beta-diketon, complex products-zinc acetylacetonate with zinc is exactly a kind of function admirable, environment-friendly high-efficiency it is thermally-stabilised
Agent, is widely applied to the stabilizer, heat stabilizer and antioxidant of all trades and professions, particularly PVC plastic.
At present, the preparation method of zinc acetylacetonate mainly has two step liquid phase methods, one-step liquid-phase reaction and solid phase method.
Two step liquid phase methods are zinc acetylacetonate synthetic methods the most traditional, are to react metal zinc salt and aqueous slkali, obtain
To zinc hydroxide solution, zinc hydroxide and acetylacetone,2,4-pentanedione reaction are then obtained into zinc acetylacetonate again.It is first that metallic zinc is soluble
Salt, which adds water, is made solution, adds certain density sodium hydroxide solution, occurs causticizing reaction production zinc hydroxide precipitation, filtering
Obtain zinc hydroxide.Zinc hydroxide and acetylacetone,2,4-pentanedione are reacted to a period of time in water again, zinc acetylacetonate precipitation is filtrated to get,
Purification obtains product.This technique distinguishing feature is to need to use substantial amounts of water twice as reaction medium, is that acetylacetone,2,4-pentanedione adds
15-20 times of dosage, can produce substantial amounts of waste water, also use aqueous slkali, and this liquid phase method has high energy consumption, and efficiency is low, dirty
Dye weight, the low shortcoming of production capacity.
One-step liquid-phase reaction is the zinc acetylacetonate synthetic method that current classics are used, and is directly to use zinc hydroxide and acetyl
Acetone reacts in aqueous medium obtains zinc acetylacetonate.Zinc hydroxide is added to the water stirring, acetylacetone,2,4-pentanedione is gradually added anti-
Should, zinc hydroxide directly reacts with acetylacetone,2,4-pentanedione in aqueous medium, is filtrated to get zinc acetylacetonate, is dried to obtain product.
This technique increases on two step liquid phase methods, does not use aqueous slkali, but still need substantial amounts of water as anti-
Medium is answered, is 10-15 times of acetylacetone,2,4-pentanedione addition, substantial amounts of waste water can be produced, this liquid phase method equally has high energy consumption, effect
Rate is low, pollution weight, the low shortcoming of production capacity.Also some companies, using methanol as reaction medium, methanol rises during the course of the reaction
To scattered effect, make acetylacetone,2,4-pentanedione and the sufficient haptoreaction of zinc hydroxide, purity can be improved.But methanol is a kind of volatile
Liquid, highly inflammable, its steam is mixed with air, can form explosive mixture, dangerous very big.Methanol also has toxicity,
Contact poisonous with skin, suction is poisonous, and harm to the human body is very big.
Solid phase method is the zinc acetylacetonate new method for producing studied in recent years.This method, which has, does not need solvent, operates
Simply, reaction speed is fast, and energy consumption is low, advantages of environment protection.Acetylacetone,2,4-pentanedione is Weak monoacid, uses solid base and acetylacetone,2,4-pentanedione
Reaction, produces the simple metal salt of acetylacetone,2,4-pentanedione, then generates zinc acetylacetonate with the complex reaction of metal zinc salt again.By solid
Alkali and acetylacetone,2,4-pentanedione are added in mill according to certain ratio to be ground, and is added a certain amount of metal zinc salt and is ground to form paste
Shape, continue griding reaction into solid powder, solid phase reaction for a period of time after, be soaked in water dissolving unreacted reactant, is filtrated to get second
Acyl acetone zinc, product is obtained after purification.
This solid phase method technique is increased compared to liquid phase method, and process water is reduced, and energy consumption is low, but stills need alkali as original
Material, finally also needs to dissolve unreacted reactant with water, it is seen that can also produce certain waste water, the unreacted reactant of residual causes product pure
Degree is not high.Mill is also possible to that abrasive media can be used, and finally also needs to separate abrasive media with product, cumbersome, no
Can efficiently it produce.
The content of the invention
The technical problem to be solved in the present invention is：Water consumption present in production technology for current zinc acetylacetonate
Greatly, high energy consumption, efficiency is low, pollution weight, and there is provided a kind of production of solid phase method under high shear acetylacetone,2,4-pentanedione for the problem of production capacity is low
The technique and its production equipment of zinc..
The technical scheme is that：A kind of solid phase method produces the technique of zinc acetylacetonate, acetylacetone,2,4-pentanedione, the compound of zinc
With water using mass ratio as 38-42%:16-24%:38-42% ratio is added in homemade high shear reaction unit, shear agitation
Reaction 1.5-2 hours, under negative pressure 0-0.1MPa, 30-60 DEG C of temperature, vacuum drying obtains zinc acetylacetonate.
The compound of described zinc is zinc hydroxide, zinc oxide or zinc carbonate.
Described water is deionized water.
Described deionized water includes ion exchange water, electrodialytic water and double distilled water.
Described high shear force reaction unit, includes the chuck of reaction vessel and its outer lining, and reaction vessel interior is provided with
Motor outside two ∑ type agitating paddles, ∑ type agitating paddle and reaction vessel is connected by decelerator with shaft joint.
Described chuck side sets steam and cooling water inlet and steam and coolant outlet.
Described two ∑ type agitating paddle flip Trims rotation.
Described ∑ type agitating paddle is ∑ type high shear differential agitating paddle, frequency control.
Temperature-measuring port is set above described reaction vessel.
Described reaction vessel is corrosion-resistant, pressure-resistant reaction vessel.
Beneficial effects of the present invention：
Present invention production zinc acetylacetonate, is the reaction that a kind of liquid-solid phase reaction is transformed into solid phase, is mixed by mechanical agitation,
Reactant acetylacetone,2,4-pentanedione and zinc hydroxide can contact the second generated at first in generation complex reaction, course of reaction under the catalysis of water
Acyl acetone zinc can wrap unreacted material, may result in the slow even reaction of reaction incomplete.It is homemade by the present invention
Powerful friction and extruding is produced between the strong shear stirring of high shear reactor, reaction mass, constantly coated particle is carried out
Broken diffusion, new reaction mass just can be contacted constantly, produce new reaction zone, generate new target product.The target of generation
Product constantly expands nucleation, ultimately forms complete reaction product --- zinc acetylacetonate.Reaction mechanism is as follows：Stirring mixing →
Shear diffusion → complex reaction → expansion nucleation → generation product.
Specifically, acetylacetone,2,4-pentanedione and metal zinc salt produce complex reaction, the acetylacetone,2,4-pentanedione of generation under the catalysis of a small amount of water
Zinc can wrap unreacted reaction mass, may result in the slow even reaction of reaction incomplete.In order that acetylacetone,2,4-pentanedione and gold
Category zinc salt fully completely attaches to reaction, and churned mechanically control is critically important, is whether whole Project Technical can be successfully crucial.
By being iteratively improved, the present invention has innovated a kind of horizontal differential Σ types Double shaft stirring reaction unit, in differential Σ type Double shaft stirrings
Under high shear forces, reaction mass generates powerful friction and extruding, and broken diffusion is constantly carried out to coated particle, and new is anti-
Answer material constantly to contact, constantly produce new reaction zone, more promote under the catalytic action of water completely reaction, in the absence of caking and
Dead angle.Therefore the high shear reaction unit designed using the present invention, the difficulty in product course of reaction is solved well, accelerates second
The complete reaction of acyl acetone zinc, the stable and reliable product quality of gained.
After reaction terminates, dry, arranged in the way of vapor by heating, vacuum as a small amount of water of catalyst in product
Go out, so while reacting complete, product is dried.Under the stirring action of high shear force, material is tentatively refined
Into coarse powder, crushed and screened finally by pulverizer, you can obtain finished product, yield is close to theoretical value.Process water is only levulinic
1-1.5 times of ketone addition, is the 1/10 of liquid phase method water consumption.
Above-mentioned production technology, not only simplify operating procedure, improve yield, reduce energy consumption and cost, reduce useless
Water process expense, more avoids pollution problem of the waste water to environment.Whole technical process does not have discharge of wastewater, realizes production work
Skill integration, can be achieved automated production after combination.Meet the policy guidance of the advanced industry of national green environmental protection.
Brief description of the drawings
Fig. 1 is reaction unit forward structure schematic diagram of the present invention；
Fig. 2 is that the present invention bows to structural representation.
Embodiment
As depicted in figs. 1 and 2, the reaction unit includes reaction vessel 4, charge door 6 and chuck 8, motor 1 and decelerator 2
Connection, decelerator 2 is connected with shaft joint 3, and shaft joint 3 is connected with the ∑ type agitating paddle 9 installed in reaction vessel 4, the stirring of ∑ type
Oar 9 is 2, and flip Trim rotates, variable ratio frequency changer speed governing；Reaction vessel 4 is acid-resistant container, and the top of reaction vessel 4 sets charging
Mouth 6, gas inlet/outlet pipe road junction 7 and temperature-measuring port 5, reaction vessel 4 is outer to set chuck 8, and the lower section of reaction vessel 4 sets discharging opening 10,
Chuck 8 sets steam and cooling water inlet 11 and steam and coolant outlet 12 sideways, can be added by steam or cooling water
Temperature or cooling.The reaction temperature of reaction vessel 4 can be conveniently measured by temperature-measuring port 5；Reaction raw materials are added instead by charge door 6
Answer in container 4, while charge door 6 is also used as service ports, after device breaks down, maintenance personal can pass through charge door
6 are overhauled into device is interior.
Embodiment 1：Reaction raw materials：Acetylacetone,2,4-pentanedione 1500g（Content 99.8%）, zinc oxide 630g（Content 99.8%）, go from
Sub- water 1800g.
First by zinc oxide and deionized water from charge door（6）It is added to reaction vessel（4）In, open agitating paddle（9）, treat
Zinc oxide is sufficiently mixed into scattered paste shape with water, is slowly added to acetylacetone,2,4-pentanedione, continues to stir, after abundant shear agitation is reacted 2 hours.
Reaction vessel is closed, steam valve and vacuum-pumping valve is opened, under negative pressure 0-0.1MPa, the lasting stirring of 30-60 DEG C of temperature
Dry 2 hours.Vapor is from gases exit line（7）Discharge, after end to be dried, steam off valve and vacuum-pumping valve.
Reacting drying terminates to obtain coarse powder, is crushed by pulverizer and obtains zinc acetylacetonate（In terms of dry product）Finished product 1931.15g, reason
By the deserved 1968.56g of calculating, net yield 98.1%
The quality index detection of zinc acetylacetonate derived above is as shown in table 1：
The product quality of the present invention of table 1
| Inspection project | Standard requirement | Examination and test of products result |
| Outward appearance | White powder | Meet the requirements |
| Zn content | 23.0-26.0 | 25.2% |
| Loss on drying（70±2℃） | ≤5.0% | 3.8% |
| Fineness | 0.25mm testing sieves pass through >=95.0 | 99.3% |
| Fusing point | 129-133℃ | 132.2℃ |
| Heavy metal | ≤0.0020% | ＜ 0.0020% |
Embodiment 2：Reaction raw materials：Acetylacetone,2,4-pentanedione 2000g（Content 99.7%）, zinc oxide 780g（Content 99.7%）, deionized water
2000g。
First by zinc hydroxide and deionized water from charge door（6）It is added to reaction vessel（4）In, open agitating paddle（9）,
Zinc to be oxidized is sufficiently mixed into scattered paste shape with water, is slowly added to acetylacetone,2,4-pentanedione, continues to stir, abundant shear agitation is reacted 2 hours
Afterwards.Reaction vessel is closed, steam valve and vacuum-pumping valve is opened, under negative pressure 0-0.1MPa, 30-60 DEG C of temperature is persistently stirred
Mix and dry 2.5 hours.Vapor is from gases exit line（7）Discharge, after end to be dried, steam off valve and vacuum pumping valve
Door.Reacting drying terminates to obtain coarse powder, is crushed by pulverizer and obtains zinc acetylacetonate（In terms of dry product）Finished product 2574.90g,
The deserved 2622.11g of theoretical calculation, net yield 98.2%
The quality index detection of zinc acetylacetonate derived above is as shown in table 2：
The product quality of the present invention of table 2
| Inspection project | Standard requirement | Examination and test of products result |
| Outward appearance | White powder | Meet the requirements |
| Zn content | 23.0-26.0% | 23.8% |
| Loss on drying（70±2℃） | ≤5.0% | 4.2% |
| Fineness | 0.25mm testing sieves pass through >=95.0 | 99.4% |
| Fusing point | 129-133℃ | 131.3℃ |
| Heavy metal | ≤0.0020% | ＜ 0.0020% |
The technique and device of zinc acetylacetonate are produced by a kind of solid phase method of the present invention, operating procedure is simplified, improves receipts
Rate, moreover it is possible to reduce energy consumption and cost, reduces wastewater treatment expense, more avoids pollution problem of the waste water to environment.Whole technique
Process does not have discharge of wastewater, realizes production technology integration, automated production can be achieved after combination, meets national green environmental protection
The policy guidance of advanced industry, has far-reaching social effect to protection China environmental resource.The zinc acetylacetonate quality of production
It is reliable and stable, it can not only meet domestic market demand, moreover it is possible to Opening International Market.Generally speaking, the research and development of the project are implemented,
With significant social and economic benefit.
Claims (10)
1. the technique that a kind of solid phase method produces zinc acetylacetonate, it is characterised in that：Acetylacetone,2,4-pentanedione, the compound of zinc and water are with quality
Than for 38-42%:16-24%:38-42% ratio is added in homemade high shear reaction unit, shear agitation reaction 1.5-2
Hour, under negative pressure 0-0.1MPa, 30-60 DEG C of temperature, vacuum drying obtains zinc acetylacetonate.
2. the technique that a kind of solid phase method according to claim 1 produces zinc acetylacetonate, it is characterised in that：Described zinc
Compound is zinc hydroxide, zinc oxide or zinc carbonate.
3. the technique that a kind of solid phase method according to claim 1 produces zinc acetylacetonate, it is characterised in that：Described water is
Deionized water.
4. the technique that a kind of solid phase method according to claim 3 produces zinc acetylacetonate, it is characterised in that：It is described go from
Sub- water includes ion exchange water, electrodialytic water and double distilled water.
5. a kind of high shear force reaction unit as claimed in claim 1, including reaction vessel（4）With the chuck of its outer lining
（8）, it is characterised in that：Reaction vessel（4）Inside is provided with two ∑ type agitating paddles（9）, ∑ type agitating paddle（9）And reaction vessel
（4）Outside motor（1）Pass through decelerator（2）With shaft joint（3）Connection.
6. high shear force reaction unit according to claim 5, it is characterised in that：Chuck（8）Side sets steam and cold
But water inlet（11）With steam and coolant outlet（12）.
7. high shear force reaction unit according to claim 5, it is characterised in that：Two ∑ type agitating paddles（9）Reversely cut
Cut rotation.
8. the high shear force reaction unit according to claim 5 or 7, it is characterised in that：Described ∑ type agitating paddle（9）For
∑ type high shear differential agitating paddle, frequency control.
9. high shear force reaction unit according to claim 5, it is characterised in that：Reaction vessel（4）Top sets thermometric
Mouthful（5）.
10. high shear force reaction unit according to claim 5, it is characterised in that：Reaction vessel（4）To be corrosion-resistant, resistance to
Press reaction vessel.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467340A (en) * | 2018-06-28 | 2018-08-31 | 湖州市菱湖新望化学有限公司 | A kind of reaction unit and its technique of solid phase method production acetylacetonate |
| CN110105184A (en) * | 2019-06-13 | 2019-08-09 | 深圳市志海实业股份有限公司 | A kind of method of Dry synthesis zinc acetylacetonate under normal pressure |
| CN110128254A (en) * | 2019-06-11 | 2019-08-16 | 东莞市汉维科技股份有限公司 | A kind of preparation process of acetylacetonate |
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|---|---|---|---|---|
| CN1299392A (en) * | 1998-03-12 | 2001-06-13 | 罗狄亚化学公司 | Use of monohydrate zinc acetylacetonate as halogenated polymer stabiliser, and prepn. method |
| JP2003342222A (en) * | 2002-05-23 | 2003-12-03 | Kanto Chem Co Inc | Method for producing zinc acetylacetonate monohydrate |
| CN101607883A (en) * | 2009-07-17 | 2009-12-23 | 湖州市菱湖新望化学有限公司 | A kind of technology of producing zinc stearate by dry method and device |
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2017
- 2017-05-27 CN CN201710391053.4A patent/CN107056597A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299392A (en) * | 1998-03-12 | 2001-06-13 | 罗狄亚化学公司 | Use of monohydrate zinc acetylacetonate as halogenated polymer stabiliser, and prepn. method |
| JP2003342222A (en) * | 2002-05-23 | 2003-12-03 | Kanto Chem Co Inc | Method for producing zinc acetylacetonate monohydrate |
| CN101607883A (en) * | 2009-07-17 | 2009-12-23 | 湖州市菱湖新望化学有限公司 | A kind of technology of producing zinc stearate by dry method and device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467340A (en) * | 2018-06-28 | 2018-08-31 | 湖州市菱湖新望化学有限公司 | A kind of reaction unit and its technique of solid phase method production acetylacetonate |
| CN108467340B (en) * | 2018-06-28 | 2024-04-30 | 湖州市菱湖新望化学有限公司 | Reaction device and process for producing acetylacetonate by solid phase method |
| CN110128254A (en) * | 2019-06-11 | 2019-08-16 | 东莞市汉维科技股份有限公司 | A kind of preparation process of acetylacetonate |
| CN110105184A (en) * | 2019-06-13 | 2019-08-09 | 深圳市志海实业股份有限公司 | A kind of method of Dry synthesis zinc acetylacetonate under normal pressure |
| CN110105184B (en) * | 2019-06-13 | 2021-08-03 | 深圳市志海实业股份有限公司 | Method for synthesizing zinc acetylacetonate by normal pressure dry method |
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