CN107266301A - A kind of isolation and purification method of acetylacetonate and its solvent used - Google Patents
A kind of isolation and purification method of acetylacetonate and its solvent used Download PDFInfo
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Abstract
A kind of isolation and purification method of acetylacetonate and its solvent used, the composition of raw materials for the solvent that the isolation and purification method is used include 30~70 parts of main solvent, 10~20 parts of secondary solvent, 0.1~1 part of solubilizer, 0.1~1 part of dispersant and 0.1~1 part of stabilizer.The isolation and purification method comprises the following steps：The first step：Described sequentially add main solvent and secondary solvent in one reaction vessel is stirred, it is to be mixed it is uniform after, dispersant, cosolvent and stabilizer are sequentially added under conditions of stirring, mixed solvent system is uniformly mixing to obtain；Second step：Acetylacetonate crude product is added in mixed solvent system made from the first step, makes the acetylacetonate dissolving crude product, solution is then filtrated to get filtrate；3rd step：The filtrate is distilled, obtained solid is pure acetylacetonate.The acetylacetone,2,4-pentanedione purity salt of separating-purifying of the present invention is up to more than 99%.
Description
Technical field
The invention belongs to the separating and purifying technology field of reaction product, and in particular to a kind of acetylacetonate is isolated and purified
Method and its solvent used.
Background technology
In the industrial production of today's society, acetylacetone,2,4-pentanedione is more and more applied due to its special structure and property
Research in terms of chemical industry, medicine, oil, the energy.Until today, by the painstaking research of numerous scientists and chemist,
A variety of acetyl acetone salts have been developed that.
The metallo-organic compound of acetylacetone,2,4-pentanedione has nowadays turned into the important Organic Ingredients of a class, due to acetylacetonate
With special structure and property, more and more applied in modern industry production in medicine, chemical industry, the energy, environment etc.
Aspect.Acetylacetonate is not only class catalyst of good performance in general production, and is also used as stabilizer, rush
Enter agent etc..In addition, acetylacetonate is also extensively used for administering the problem of environmental pollution that modern Economy Development is brought.
Current environmental protection to China has great importance.
According to Recent Research both domestic and external so far, liquid phase method and solid phase method are topmost as acetylacetonate
Synthetic method, wherein the most commonly used with liquid phase method.It can be seen that acetylacetone,2,4-pentanedione is Weak monoacid by the structure of acetylacetone,2,4-pentanedione.It is so-called
Industrially conventional liquid phase method allow it to occur acid-base neutralization reaction with hydroxide using the property of acetylacetone,2,4-pentanedione, and hydroxide
Thing precipitation is obtained generally by aqueous slkali and soluble metal reactant salt.
It can be seen that liquid phase method production acetylacetonate often produces hydroxide precipitation and metal oxide impurities are mixed
Together in acetylacetonate, the purity generation to acetylacetonate has a strong impact on.
The content of the invention
Present invention aims at the solvent for providing a kind of isolation and purification method of acetylacetonate and its using.
To achieve the above object, the technical scheme that provides of the present invention is：A kind of acetylacetonate isolates and purifies what is used
Solvent, the composition of raw materials of the solvent includes the component of following mass parts：
The mass parts of main solvent 30~70；
The mass parts of secondary solvent 10~20；
The mass parts of solubilizer 0.1~1；
The mass parts of dispersant 0.1~1；
The mass parts of stabilizer 0.1~1；
The main solvent is phenmethylol, toluene, methanol, ethanol, benzene, dichloromethane, ethyl acetate, n-butanol, isobutanol, positive heptan
One kind, two or more combination in alkane, ethylene glycol, dimethylbenzene, dipentene, hexamethylene；The secondary solvent is third
One kind, two or more combination in ketone, MEK, cyclohexanone, methyl cyclohexanone, butanone, ether, butyl ether；It is described
Solubilizer is in Tweens surfactant, spans surfactant, polyoxyethylene fatty acid, neopelex
A kind of, two or more combination；The dispersant is lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, poly-
One kind, two or more combination in acrylamide, polyethylene glycol；The stabilizer is light stabilizer NBC, light stabilization
Agent 2002, light stabilizer 770, light stabilizer 901, light stabilizer GW-540, pentaerythrite, xylitol, one kind in mannitol,
Two or more combination.
It is preferred that technical scheme be：The Tweens surfactant is Tween 20（Polyethenoxy sorbitan list
Laurate）、Tween 40（Polyethenoxy sorbitan monopalmitate）、Tween 60（Polyethenoxy sorbitan
Monostearate）、Tween 80（Polyoxyethylene sorbitan monooleate）、Tween 85（Polyethenoxy sorbitan
Trioleate）.
It is preferred that technical scheme be：The spans surfactant is Span20（Arlacel-20）、
Span40（Arlacel-40）、 Span60（Arlacel-60）、Span80（Anhydro sorbitol
Monoleate）、Span85（Sorbitan trioleate）
To achieve the above object, the technical scheme that provides of the present invention is：A kind of isolation and purification method of acetylacetonate, described point
The composition of raw materials of the solvent used from purification process includes the component of following mass parts：
The mass parts of main solvent 30~70；
The mass parts of secondary solvent 10~20；
The mass parts of solubilizer 0.1~1；
The mass parts of dispersant 0.1~1；
The mass parts of stabilizer 0.1~1；
The main solvent is phenmethylol, toluene, methanol, ethanol, benzene, dichloromethane, ethyl acetate, n-butanol, isobutanol, positive heptan
One kind, two or more combination in alkane, ethylene glycol, dimethylbenzene, dipentene, hexamethylene；The secondary solvent is third
One kind, two or more combination in ketone, MEK, cyclohexanone, methyl cyclohexanone, butanone, ether, butyl ether；It is described
Solubilizer is in Tweens surfactant, spans surfactant, polyoxyethylene fatty acid, neopelex
A kind of, two or more combination；The dispersant is lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, poly-
One kind, two or more combination in acrylamide, polyethylene glycol；The stabilizer is light stabilizer NBC, light stabilization
Agent 2002, light stabilizer 770, light stabilizer 901, light stabilizer GW-540, pentaerythrite, xylitol, one kind in mannitol,
Two or more combination；
The isolation and purification method comprises the following steps：
The first step：Described sequentially add main solvent and secondary solvent in one reaction vessel is stirred, it is to be mixed it is uniform after, in stirring
Under conditions of sequentially add dispersant, cosolvent and stabilizer, be uniformly mixing to obtain mixed solvent system；
Second step：Acetylacetonate crude product is added in mixed solvent system made from the first step, makes the acetylacetonate thick
Product are dissolved, and solution then is filtrated to get into filtrate；
3rd step：The filtrate is distilled, obtained solid is pure acetylacetonate.
It is preferred that technical scheme be：The temperature conditionss of the first step are 20 ~ 95 DEG C.
It is preferred that technical scheme be：The temperature conditionss of the second step are 20 ~ 95 DEG C.
It is preferred that technical scheme be：The temperature conditionss of 3rd step are 100 ~ 200 DEG C.
It is preferred that technical scheme be：The Tweens surfactant be Tween 20, Tween 40, Tween 60,
Tween 80、Tween 85。
It is preferred that technical scheme be：The spans surfactant be Span20, Span40, Span60, Span80,
Span85。
It is preferred that technical scheme be：In the 3rd step, distill obtained mother liquor and used as mixed solvent system.
Cellulose derivative is that the life after esterification or etherification reaction occurs with the hydroxyl in cellulosic molecule and chemical reagent
Into thing.Cellulose derivative can be divided into cellulose ether and cellulose esters and fiber according to the design feature of reaction product
Plain ether-ether three major types.The cellulose esters of practical application has：Cellulose nitrate, cellulose ethanoate, cellulose acetate butyric acid
Ester and cellulose sulfonate.Cellulose ethers has：Methylcellulose, carboxymethyl cellulose, ethyl cellulose, hydroxy ethyl fiber
Element, cyanethyl cellulose, hydroxypropyl cellulose and hydroxypropyl methyl cellulose etc..In addition, also ester ether mixed derivative.
Acetylacetonate include calcium acetylacetonate, aluminium acetylacetonate, acetylacetone cobalt, nickel acetylacetonate, acetylacetone copper,
The acetylacetone,2,4-pentanediones such as zinc acetylacetonate, ferric acetyl acetonade, chromium acetylacetonate, titanium acetylacetone, manganese acetylacetonate, acetylacetone,2,4-pentanedione potassium gold
Belong to salt.
Because above-mentioned technical proposal is used, the present invention this have the advantage that compared with prior art：
1st, the present invention is dissolved in mixing by the ratio of main solvent and secondary solvent in adjusting solvent system using acetylacetonate
Dicyandiamide solution, and the undissolved feature of impurity, reach the purpose isolated and purified, effect is good, cost is low, product with isolating and purifying
The high advantage of the rate of recovery, and the quality of product is not influenceed.
2nd, present invention process flow and principle is easy and effective, raw material and method green non-pollution, is conducive to green production.Behaviour
Make flow easily controllable, available for mass producing.
3rd, the acetylacetone,2,4-pentanedione purity salt of separating-purifying of the present invention is up to more than 99%.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
Embodiment 1, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of isolation and purification method of acetylacetonate, is prepared from by the component raw material of following weight：
The mass parts of calcium acetylacetonate crude product 20：Main solvent：The mass parts of phenmethylol 39；The mass parts of toluene 20；Secondary solvent：Acetone 20
Mass parts；Solubilizer：The mass parts of lauryl sodium sulfate 0.4；Dispersant：The mass parts of polyethylene glycol 0.3；Stabilizer：Light is stable
The mass parts of agent 2,002 0.3.
Its preparation method comprises the following steps：
（1）Dispensing：According to formula metering each component.
（2）Prepare a mixed solvent system：At 50 DEG C, phenmethylol, methanol and acetone are sequentially added in reactor
Stirring, after being sufficiently mixed, sequentially adds polysorbate, polyethylene glycol and light stabilizer 2002, fully under conditions of stirring
Stirring.
（3）At 50 DEG C, a certain amount of calcium acetylacetonate crude product is added into mixed solvent system, under conditions of stirring,
Dissolve after 12 hours, solution is filtered, resulting insoluble solid is weighed after drying.
（4）Liquid obtained by filtering is distilled under the conditions of 200 DEG C, obtained solid is pure acetylacetone,2,4-pentanedione
Calcium, and mother liquor can be then continuing with as mixed solvent system.
（5）Acetylacetonate can finally be obtained and be dissolved in mixed solvent, and impurity is then completely insoluble in mixed solvent, then can lead to
Mixed solvent is crossed to isolate and purify acetylacetonate from impurity.
Embodiment 2, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of isolation and purification method of acetylacetonate, is prepared from by the component raw material of following weight：
Zinc acetylacetonate crude product 20：Main solvent：Phenmethylol 39；Methanol 20；Secondary solvent：Acetone 20；Solubilizer：Polysorbate
0.4；Dispersant：Polyacrylamide 0.3；Stabilizer：Light stabilizer NBC 0.3.
Its preparation method comprises the following steps：
（1）Dispensing：According to formula metering each component.
（2）Prepare a mixed solvent system：At 50 DEG C, phenmethylol, methanol and acetone are sequentially added in reactor
Stirring, after being sufficiently mixed, polysorbate, polyethylene glycol and light stabilizer NBC is sequentially added under conditions of stirring, is fully stirred
Mix.
（3）At 50 DEG C, a certain amount of zinc acetylacetonate crude product is added into mixed solvent system, under conditions of stirring,
Dissolve after 12 hours, solution is filtered, resulting insoluble solid is weighed after drying.
（4）Liquid obtained by filtering is distilled under the conditions of 200 DEG C, obtained solid is pure acetylacetone,2,4-pentanedione
Zinc, and mother liquor can be then continuing with as mixed solvent system.
（5）Acetylacetonate can finally be obtained and be dissolved in mixed solvent, and impurity is then completely insoluble in mixed solvent, then can lead to
Mixed solvent is crossed to isolate and purify acetylacetonate from impurity.
Embodiment 3, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of isolation and purification method of acetylacetonate, is prepared from by the component raw material of following weight：
The mass parts of magnesium acetylacetonate crude product 20：Main solvent：The mass parts of ethanol 39；The mass parts of dichloromethane 20；Secondary solvent：Acetone
20 mass parts；Solubilizer：The mass parts of polysorbate 0.4；Dispersant：The mass parts of polyethylene glycol 0.3；Stabilizer：Light stabilizer NBC
0.3 mass parts.
Its preparation method comprises the following steps：
（1）Dispensing：According to formula metering each component.
（2）Prepare a mixed solvent system：At 50 DEG C, ethanol, dichloromethane and acetone are sequentially added into reactor
Middle stirring, after being sufficiently mixed, sequentially adds polysorbate, polyethylene glycol and light stabilizer NBC, fully under conditions of stirring
Stirring.
（3）At 50 DEG C, a certain amount of magnesium acetylacetonate crude product is added into mixed solvent system, under conditions of stirring,
Dissolve after 12 hours, solution is filtered, resulting insoluble solid is weighed after drying.
（4）Liquid obtained by filtering is distilled under the conditions of 200 DEG C, obtained solid is pure acetylacetone,2,4-pentanedione
Magnesium, and mother liquor can be then continuing with as mixed solvent system.
（5）Acetylacetonate can finally be obtained and be dissolved in mixed solvent, and impurity is then completely insoluble in mixed solvent, then can lead to
Mixed solvent is crossed to isolate and purify acetylacetonate from impurity.
Embodiment 4, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of isolation and purification method of acetylacetonate, is prepared from by the component raw material of following weight：
The mass parts of aluminium acetylacetonate crude product 20：Main solvent：The mass parts of phenmethylol 29；The mass parts of ethyl acetate 30；Secondary solvent：First
The mass parts of pentylcyclohexanone 20；Solubilizer：The mass parts of polysorbate 0.4；Dispersant：The mass parts of methyl anyl alcohol 0.3；Stabilizer：Light
The mass parts of stabilizer NBC 0.3.
Its preparation method comprises the following steps：
（1）Dispensing：According to formula metering each component.
（2）Prepare a mixed solvent system：At 50 DEG C, phenmethylol, ethyl acetate and acetone are sequentially added into reaction
Stirred in device, after being sufficiently mixed, polysorbate, polyethylene glycol and light stabilizer NBC are sequentially added under conditions of stirring, is filled
Divide stirring.
（3）At 50 DEG C, a certain amount of aluminium acetylacetonate crude product is added into mixed solvent system, under conditions of stirring,
Dissolve after 12 hours, solution is filtered, resulting insoluble solid is weighed after drying.
（4）Liquid obtained by filtering is distilled under the conditions of 200 DEG C, obtained solid is pure acetylacetone,2,4-pentanedione
Aluminium, and mother liquor can be then continuing with as mixed solvent system.
（5）Acetylacetonate can finally be obtained and be dissolved in mixed solvent, and impurity is then completely insoluble in mixed solvent, then can lead to
Mixed solvent is crossed to isolate and purify acetylacetonate from impurity.
Embodiment 5, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of isolation and purification method of acetylacetonate, is prepared from by the component raw material of following weight：
The mass parts of acetylacetone copper crude product 20：Main solvent：The mass parts of phenmethylol 29；The mass parts of benzene 30；Secondary solvent：The matter of acetone 20
Measure part；Solubilizer：The mass parts of polyoxyethylene fatty acid 0.4；Dispersant：The mass parts of polyethylene glycol 0.3；Stabilizer：Light stabilizer
The mass parts of NBC 0.3.
Its preparation method comprises the following steps：
（1）Dispensing：According to formula metering each component.
（2）Prepare a mixed solvent system：At 50 DEG C, phenmethylol, benzene and acetone are sequentially added in reactor and stirred
Mix, after being sufficiently mixed, sorbitan fatty acid ester, polyethylene glycol and light stabilizer are sequentially added under conditions of stirring
NBC, is sufficiently stirred for.
（3）At 50 DEG C, a certain amount of acetylacetone copper crude product is added into mixed solvent system, under conditions of stirring,
Dissolve after 12 hours, solution is filtered, resulting insoluble solid is weighed after drying.
（4）Liquid obtained by filtering is distilled under the conditions of 200 DEG C, obtained solid is pure acetylacetone,2,4-pentanedione
Copper, and mother liquor can be then continuing with as mixed solvent system.
（5）Acetylacetonate can finally be obtained and be dissolved in mixed solvent, and impurity is then completely insoluble in mixed solvent, then can lead to
Mixed solvent is crossed to isolate and purify acetylacetonate from impurity.
Embodiment 6, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of isolation and purification method of acetylacetonate, is prepared from by the component raw material of following weight：
The mass parts of ferric acetyl acetonade crude product 20：Main solvent：The mass parts of dichloromethane 29；The mass parts of benzene 30；Secondary solvent：Ether 20
Mass parts；Solubilizer：The mass parts of sorbitan fatty acid ester 0.4；Dispersant：The mass parts of polyethylene glycol 0.3；Stabilizer：Light
The mass parts of stabilizer 770 0.3.
Its preparation method comprises the following steps：
（1）Dispensing：According to formula metering each component.
（2）Prepare a mixed solvent system：At 50 DEG C, dichloromethane, benzene and acetone are sequentially added in reactor
Stirring, after being sufficiently mixed, sequentially adds sorbitan fatty acid ester, polyethylene glycol and light stabilizer under conditions of stirring
770, it is sufficiently stirred for.
（3）At 50 DEG C, a certain amount of ferric acetyl acetonade crude product is added into mixed solvent system, under conditions of stirring,
Dissolve after 12 hours, solution is filtered, resulting insoluble solid is weighed after drying.
（4）Liquid obtained by filtering is distilled under the conditions of 200 DEG C, obtained solid is pure acetylacetone,2,4-pentanedione
Iron, and mother liquor can be then continuing with as mixed solvent system.
（5）Acetylacetonate can finally be obtained and be dissolved in mixed solvent, and impurity is then completely insoluble in mixed solvent, then can lead to
Mixed solvent is crossed to isolate and purify acetylacetonate from impurity.
Embodiment 7, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of acetylacetonate isolates and purifies the solvent used, and the composition of raw materials of the solvent includes the group of following mass parts
Point：
The mass parts of main solvent 70；
The mass parts of secondary solvent 10；
The mass parts of solubilizer 0.1；
The mass parts of dispersant 0.1；
The mass parts of stabilizer 0.1；
The main solvent is by phenmethylol, methanol, ethanol according to 1：1：1 volume ratio mixing is constituted；The secondary solvent by acetone,
MEK, cyclohexanone are according to 1：2：1 volume ratio mixing is constituted；The solubilizer is by Tween 20 and Span40 according to 1：1
Volume ratio mixing is constituted.The dispersant is by lauryl sodium sulfate, methyl anyl alcohol, polyacrylamide, poly- second two according to 1：
0.5：2：1 mass ratio mixing is constituted；The stabilizer is by light stabilizer NBC and light stabilizer 2002 according to 1：2 mass ratio
Example mixing is constituted.
The isolation and purification method comprises the following steps：
The first step：Described sequentially add main solvent and secondary solvent in one reaction vessel is stirred, it is to be mixed it is uniform after, in stirring
Under conditions of sequentially add dispersant, cosolvent and stabilizer, be uniformly mixing to obtain mixed solvent system；
Second step：Acetylacetonate crude product is added in mixed solvent system made from the first step, makes the acetylacetonate thick
Product are dissolved, and solution then is filtrated to get into filtrate；
3rd step：The filtrate is distilled, obtained solid is pure acetylacetonate.
The temperature conditionss of the first step are 20 DEG C.
The temperature conditionss of the second step are 20 DEG C.
The temperature conditionss of 3rd step are 110 DEG C.
In the 3rd step, distill obtained mother liquor and used as mixed solvent system.
Embodiment 8, a kind of isolation and purification method of acetylacetonate and its solvent used
A kind of acetylacetonate isolates and purifies the solvent used, and the composition of raw materials of the solvent includes the group of following mass parts
Point：
The mass parts of main solvent 70；
The mass parts of secondary solvent 20；
The mass parts of solubilizer 1；
The mass parts of dispersant 1；
The mass parts of stabilizer 1；
The main solvent is by ethylene glycol and hexamethylene according to 1：The combination that 3 volume ratio is constituted；The secondary solvent by ether and
Butyl ether is according to 1:The combination that 1 volume ratio is constituted；The solubilizer is pressed by polyoxyethylene fatty acid and neopelex
According to 5：The combination that 1 mass ratio is constituted；The dispersant is by cellulose nitrate and carboxymethyl cellulose according to 1：1 mass ratio is constituted
Combination；The stabilizer is pentaerythrite, xylitol, mannitol according to 1：2：The combination that 5 mass ratio is constituted.
The isolation and purification method comprises the following steps：
The first step：Described sequentially add main solvent and secondary solvent in one reaction vessel is stirred, it is to be mixed it is uniform after, in stirring
Under conditions of sequentially add dispersant, cosolvent and stabilizer, be uniformly mixing to obtain mixed solvent system；
Second step：Acetylacetonate crude product is added in mixed solvent system made from the first step, makes the acetylacetonate thick
Product are dissolved, and solution then is filtrated to get into filtrate；
3rd step：The filtrate is distilled, obtained solid is pure acetylacetonate.
The temperature conditionss of the first step are 95 DEG C.
The temperature conditionss of the second step are 95 DEG C.
The temperature conditionss of 3rd step are 200 DEG C.
In the 3rd step, distill obtained mother liquor and used as mixed solvent system.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of acetylacetonate isolates and purifies the solvent used, it is characterised in that：Under the composition of raw materials of the solvent includes
State the component of mass parts：
The mass parts of main solvent 30~70；
The mass parts of secondary solvent 10~20；
The mass parts of solubilizer 0.1~1；
The mass parts of dispersant 0.1~1；
The mass parts of stabilizer 0.1~1；
The main solvent is phenmethylol, toluene, methanol, ethanol, benzene, dichloromethane, ethyl acetate, n-butanol, isobutanol, positive heptan
One kind, two or more combination in alkane, ethylene glycol, dimethylbenzene, dipentene, hexamethylene；The secondary solvent is third
One kind, two or more combination in ketone, MEK, cyclohexanone, methyl cyclohexanone, butanone, ether, butyl ether；It is described
Solubilizer is in Tweens surfactant, spans surfactant, polyoxyethylene fatty acid, neopelex
A kind of, two or more combination；The dispersant is lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, poly-
One kind, two or more combination in acrylamide, polyethylene glycol；The stabilizer is light stabilizer NBC, light stabilization
Agent 2002, light stabilizer 770, light stabilizer 901, light stabilizer GW-540, pentaerythrite, xylitol, one kind in mannitol,
Two or more combination.
2. acetylacetonate according to claim 1 isolates and purifies the solvent used, it is characterised in that：The Tweens
Surfactant is Tween 20, Tween 40, Tween 60, Tween 80, Tween 85.
3. acetylacetonate according to claim 1 isolates and purifies the solvent used, it is characterised in that：The spans
Surfactant is Span20, Span40, Span60, Span80, Span85.
4. a kind of isolation and purification method of acetylacetonate, it is characterised in that：The original for the solvent that the isolation and purification method is used
Material formula includes the component of following mass parts：
The mass parts of main solvent 30~70；
The mass parts of secondary solvent 10~20；
The mass parts of solubilizer 0.1~1；
The mass parts of dispersant 0.1~1；
The mass parts of stabilizer 0.1~1；
The main solvent is phenmethylol, toluene, methanol, ethanol, benzene, dichloromethane, ethyl acetate, n-butanol, isobutanol, positive heptan
One kind, two or more combination in alkane, ethylene glycol, dimethylbenzene, dipentene, hexamethylene；The secondary solvent is third
One kind, two or more combination in ketone, MEK, cyclohexanone, methyl cyclohexanone, butanone, ether, butyl ether；It is described
Solubilizer is in Tweens surfactant, spans surfactant, polyoxyethylene fatty acid, neopelex
A kind of, two or more combination；The dispersant is lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, poly-
One kind, two or more combination in acrylamide, polyethylene glycol；The stabilizer is light stabilizer NBC, light stabilization
Agent 2002, light stabilizer 770, light stabilizer 901, light stabilizer GW-540, pentaerythrite, xylitol, one kind in mannitol,
Two or more combination；
The isolation and purification method comprises the following steps：
The first step：Described sequentially add main solvent and secondary solvent in one reaction vessel is stirred, it is to be mixed it is uniform after, in stirring
Under conditions of sequentially add dispersant, cosolvent and stabilizer, be uniformly mixing to obtain mixed solvent system；
Second step：Acetylacetonate crude product is added in mixed solvent system made from the first step, makes the acetylacetonate thick
Product are dissolved, and solution then is filtrated to get into filtrate；
3rd step：The filtrate is distilled, obtained solid is pure acetylacetonate.
5. the isolation and purification method of acetylacetonate according to claim 4, it is characterised in that：The temperature of the first step
Condition is 20 ~ 95 DEG C.
6. the isolation and purification method of acetylacetonate according to claim 4, it is characterised in that：The temperature of the second step
Condition is 20 ~ 95 DEG C.
7. the isolation and purification method of acetylacetonate according to claim 4, it is characterised in that：The temperature of 3rd step
Condition is 100 ~ 200 DEG C.
8. the isolation and purification method of acetylacetonate according to claim 4, it is characterised in that：Live on the Tweens surface
Property agent be Tween 20, Tween 40, Tween 60, Tween 80, Tween 85.
9. the isolation and purification method of acetylacetonate according to claim 4, it is characterised in that：Live on the spans surface
Property agent be Span20, Span40, Span60, Span80, Span85.
10. the isolation and purification method of acetylacetonate according to claim 4, it is characterised in that：In the 3rd step,
Obtained mother liquor is distilled to use as mixed solvent system.
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| CN109776857B (en) * | 2018-12-24 | 2020-10-27 | 厦门大学 | Plasma plastic degradation device and degradation solution formula thereof |
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