CN109912734A - A kind of production method of low ash component polypropylene resin - Google Patents
A kind of production method of low ash component polypropylene resin Download PDFInfo
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Abstract
The present invention proposes a kind of production method of low ash component polypropylene resin, belongs to the field of production of resin.The production method includes the following steps: a) once washing: raw material acrylic resin to be processed being put into washing kettle, the mixing lotion one being made of hydrocarbon solvent and complexing agent is added, after heating, closed stirring, centrifugal discharge obtains hard resin material one；B) secondary washing: being added the mixing lotion two being made of hydrocarbon solvent, complexing agent and alcohols solvent, and centrifugal discharge obtains hard resin material two；C) it washs three times: the mixing lotion three being made of complexing agent and alcohols solvent is added, after heating, closed stirring, centrifugal discharge obtains hard resin material three；D) four washings: being added alcohols solvent, and centrifugal discharge obtains hard resin material four.This method is not necessarily to individually designed exploitation catalyst, simple and easy without changing polymerization process, reduces production cost, and the acrylic resin base-material suitable for the production of various techniques carries out deep cleaning.
Description
Technical field
The present invention relates to the field of production of resin, especially a kind of production method of low ash component polypropylene resin.
Background technique
Polypropylene is a kind of thermoplastic resin as obtained by propylene polymerization, because it is with low loss factor and high volume resistance
Coefficient can be used for electrical field, such as capacitor film.Content of ashes is important measurement index in acrylic resin, ash
Divide and is mainly derived from the major catalyst titanium tetrachloride (TiCl selected in polymerization reaction4), carrier magnesium dichloride (MgCl2), co-catalysis
Agent triethyl aluminum (Al (Et)3) and silanes external electron donor, the titanium generated, magnesium, aluminium, silicon are the main components of ash content.One
As for, the content of ashes of acrylic resin used by electrical field requires to be lower than 50ppm.
Usually there are mainly two types of methods for preparation low ash component polypropylene resin.One is by designing special catalyst, gather
Conjunction obtains satisfactory acrylic resin.For example, Chinese patent 201310473291.1 discloses a kind of low ash component polypropylene
The synthetic method of wire drawing PP Pipe Compound resin adds or is not added external electron donor few under major catalyst and co-catalyst effect
Under the conditions of, propylene carries out exclusive reaction in two sections of annular-pipe reactors and generates polypropylene base-material, by acrylic resin base-material and antioxygen
Agent mixing, obtains low-ash acrylic resin product, and ash content is less than 100ppm.For another example, Chinese patent 201310488478.9
A kind of electrical membrane method for preparing polypropylene resin is disclosed, using the catalyst of high activity, high vertical structure directionality, by catalyst
Each component carries out pre-contact reaction, and pre-contact reaction product and olefinic polymerization monomer are preferably carried out prepolymerization, then carry out third
Alkene polymerization reaction obtains the acrylic resin that a kind of ash content is low, molecular weight distribution is wider, high mechanical strength and tensile property are good,
Its content of ashes is in 50ppm or less.However, the individually designed exploitation catalyst applicable craft production of the process requirement.
Another kind removes ash content by changing washing methods, produces the acrylic resin of low ash content.For example, China is specially
Benefit 201710762015.5 discloses a kind of insoluble macromolecule resin washing methods of water, and material resin passes through water and acid elution, so
PH is adjusted to 10 or more with nonmetallic alkali or nonmetallic salt of weak acid afterwards, then discharging dehydration, obtains low ash and divide naval stores.So
And resin content of ashes obtained by this method is relatively high.
Summary of the invention
The present invention proposes a kind of method for producing low ash component polypropylene resin, by adjusting cleaning solvent and washing accordingly
Method is washed, the cleaning solvent of different compound systems is formed using hydrocarbon solvent, complexing agent, alcohols solvent etc., through multistep washers
Skill removes acrylic resin ash content, while improving polypropylene resin isotactic degree, and resin is made to be more suitable for electrical field.
The present invention proposes a kind of production method of low ash component polypropylene resin, including to raw material acrylic resin to be processed into
Row washing, the washing include the following steps:
A) once washing: raw material acrylic resin to be processed is put into washing kettle, is added by hydrocarbon solvent and complexing agent
The mixing lotion one of composition, after heating, closed stirring, centrifugal discharge obtains hard resin material one；
B) secondary washing: step a) obtained solid resin material one is put into washing kettle, is added by hydrocarbon solvent, complexing
The mixing lotion two of agent and alcohols solvent composition, after heating, closed stirring, centrifugal discharge obtains hard resin material two；
C) it washs three times: step b) obtained solid resin material two is put into washing kettle, be added by complexing agent and alcohols
The mixing lotion three of solvent composition, after heating, closed stirring, centrifugal discharge obtains hard resin material three；
D) four washings: step c) obtained solid resin material three is put into washing kettle, and alcohols solvent, heating is added
Afterwards, closed stirring, centrifugal discharge obtain hard resin material four.
Further, content of ashes≤50ppm of final obtained solid resin material four.
Further, the method also includes step e): after step d), repeating step c)-d).
Further, the hydrocarbon solvent includes the mixing of one or both of alkane and aromatic hydrocarbon, wherein the alkane
The carbon atom number of hydrocarbon is 5-20；Preferably, the alkane include pentane, it is isopentane, n-hexane, normal heptane, normal octane, different pungent
The mixing of one or more of alkane, n -nonane, n-decane, the aromatic hydrocarbon include toluene, ethylbenzene, dimethylbenzene, front three
The mixing of one or more of benzene.
Further, complexing agent includes acetylacetone,2,4-pentanedione, ethylenediamine tetra-acetic acid (EDTA), oxalic acid, tartaric acid, malonic acid, lemon
The mixing of one or more of lemon acid, preferably acetylacetone,2,4-pentanedione.
Further, alcohols solvent include methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, amylalcohol, hexanol, 2- methyl anyl alcohol,
The mixing of one or more of 2- ethyl butanol, enanthol, 2-Ethylhexyl Alcohol, octanol and decyl alcohol.
Further, in step a), the additive amount of hydrocarbon solvent is 5-20 times of raw material acrylic resin quality, complexing agent
Additive amount be 3-15 times of raw material acrylic resin quality.
Further, in step b), the additive amount of hydrocarbon solvent is 4-16 times of raw material acrylic resin quality, complexing agent
Additive amount be 5-10 times of raw material acrylic resin quality, the additive amount of alcohols solvent for raw material acrylic resin quality 3-
18 times.
Further, in step c), the additive amount of complexing agent is 4-8 times of raw material acrylic resin, and alcohols solvent adds
Dosage is 5-15 times of raw material acrylic resin.
Further, in step d), the additive amount of alcohols solvent is 5-15 times of raw material acrylic resin.
Further, step a)-d), being warming up to temperature is 60-140 DEG C, and the time of stirring is 0.2-4 hours.
Further, the method also includes step f): by the drying of final obtained solid resin material four, crushing, packaging
Obtain product.
The production method of low ash component polypropylene resin provided by the present invention has the advantage that
The present invention is by adjusting cleaning solvent and corresponding washing methods, using hydrocarbon solvent, complexing agent, alcohols solvent
Etc. the cleaning solvent for forming different compound systems, through multistep washing process, acrylic resin ash content is removed, to reduce polypropylene
The content of ashes of resin, while isotacticity is promoted, production more meets the acrylic resin of electrician's production requirement.With prior art phase
Than, this method is not necessarily to individually designed exploitation catalyst, and it is simple and easy without changing polymerization process, reduce production cost.
Meanwhile to the various resin binders for not meeting the requirement of acrylic resin ash content degree, it can carry out removing ash content and reach requirement, and
Preferable removal effect is all had to each inorganic elements in ash content.Moreover, hydrocarbon solvent can also elution fraction random polypropylene,
Product isotacticity is improved, making gained resin, it is more suitable for electrical field.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
The embodiment of the present invention proposes a kind of production method of low ash component polypropylene resin, includes the following steps:
A) once washing: raw material acrylic resin to be processed is put into washing kettle, is added by hydrocarbon solvent and complexing agent
The mixing lotion one of composition, after heating, closed stirring, centrifugal discharge obtains hard resin material one；
B) secondary washing: step a) obtained solid resin material one is put into washing kettle, is added by hydrocarbon solvent, complexing
The mixing lotion two of agent and alcohols solvent composition, after heating, closed stirring, centrifugal discharge obtains hard resin material two；
C) it washs three times: step b) obtained solid resin material two is put into washing kettle, be added by complexing agent and alcohols
The mixing lotion three of solvent composition, after heating, closed stirring, centrifugal discharge obtains hard resin material three；
D) four washings: step c) obtained solid resin material three is put into washing kettle, and alcohols solvent, heating is added
Afterwards, closed stirring, centrifugal discharge obtain hard resin material four.
Polypropylene can be used for electrical field because it is with low loss factor and high specific volume resistance.In general, being used for
The acrylic resin of electrical field, content of ashes need to be lower than 50ppm.In the prior art, acrylic resin content of ashes is reduced
It is a kind of to need individually designed catalyst there are mainly two types of method, corresponding polymerization process is designed, it is complicated for operation；Another kind is logical
Change washing methods removing ash content is crossed, reduces content of ashes in acrylic resin, but this method reduction resin content of ashes is limited, washes
It is still higher to wash rear content of ashes, and isotacticity is lower, is not suitable for electrical field.
The present invention is by adjusting cleaning solvent and corresponding washing methods, using hydrocarbon solvent, complexing agent, alcohols solvent
Etc. the cleaning solvent for forming different compound systems, through multistep washing process, acrylic resin ash content is removed, to reduce polypropylene
The content of ashes of resin, while isotacticity is promoted, production more meets the acrylic resin of electrician's production requirement.
In the present invention, the mixing lotion one that once washing is formed using hydrocarbon solvent and complexing agent can make resin swelling, just
Enter in resin in hydrocarbon solvent etc.；The mixing lotion two that secondary washing is formed using hydrocarbon solvent, complexing agent and alcohols solvent,
The main characteristic dissolved each other using hydrocarbon solvent and complexing agent, makes it into resin inner complexation aluminium element etc., while alcohols solvent
It can also be brought into resin by hydrocarbon solvent, be conducive to washing；Washing is mainly using alcohols solvent elution titanium, magnesium etc. three times, and takes away
Complexing agent and hydrocarbon solvent；Alcohols solvent is used alone in four washings, can be sufficiently impregnated removing impurity in resin, and be easy to
Later period is dry.
This method is not necessarily to individually designed exploitation catalyst, simple and easy without changing polymerization process, reduces production
Cost.Meanwhile to the various resin binders for not meeting acrylic resin content of ashes requirement, it can carry out deliming and reach requirement,
And preferable removal effect is all had to each inorganic elements such as titanium, aluminium, magnesium and silicon etc. in ash content, it is applied widely.Moreover, also
Random polypropylene can be eluted, product isotacticity is improved, making gained resin, it is more suitable for electrical field.
The present invention is produced suitable for slurry polymerization, bulk polymerization, ontology-various techniques such as gas phase combination and gas-phase polymerization
Acrylic resin base-material carries out deep cleaning.
In an embodiment of the present invention, content of ashes≤50ppm of final obtained solid resin material four.Acrylic resin
Content of ashes is lower than 50ppm, is suitable for electrical field application.
In an embodiment of the present invention, after step d), step c)-d is repeated), further decrease obtained solid tree
The content of ashes of rouge material is allowed to lower than 50ppm.After four washings, washing and four washings, are relied primarily in triplicate
Complexing agent is eluted with alcohols solvent, to achieve the purpose that further to remove ash content in resin.
Specifically, repeat step c)-d) number be 0-10 times.It is specifically as follows 0,1,2,3,4,5 etc..
In an embodiment of the present invention, hydrocarbon solvent includes the mixing of one or both of alkane and aromatic hydrocarbon；Wherein,
The carbon atom number of alkane is 5-20；
Preferably, alkane includes pentane, isopentane, n-hexane, normal heptane, normal octane, isooctane, n -nonane, the positive last of the ten Heavenly stems
The mixing of one or more of alkane；Aromatic hydrocarbon include one or both of toluene, ethylbenzene, dimethylbenzene, trimethylbenzene with
On mixing；
It is furthermore preferred that alkane includes the mixing of one or more of isopentane, n-hexane, isooctane, n-decane；
Aromatic hydrocarbon includes the mixing of one or both of toluene, ethylbenzene.
In a preferred embodiment, hydrocarbon solvent can be alkane, or aromatic hydrocarbon, or alkane
With two kinds of combination of aromatic hydrocarbon.In the embodiment of the present invention, hydrocarbon solvent is conducive to elute random polypropylene, improves product isotactic
Degree.
In an embodiment of the present invention, complexing agent include acetylacetone,2,4-pentanedione, ethylenediamine tetra-acetic acid (EDTA), oxalic acid, tartaric acid,
The mixing of one or more of malonic acid, citric acid, preferably acetylacetone,2,4-pentanedione.
In an embodiment of the present invention, alcohols solvent include methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, amylalcohol, hexanol,
The mixing of one or more of 2- methyl anyl alcohol, 2- ethyl butanol, enanthol, 2-Ethylhexyl Alcohol, octanol and decyl alcohol.It is preferred that
, alcohols solvent includes the mixing of one or more of ethyl alcohol, isopropanol, amylalcohol, enanthol.
In an embodiment of the present invention, in step a), the content of ashes of raw material acrylic resin to be processed is higher than 50ppm；
Preferably, the content of ashes of raw material acrylic resin to be processed is 50-200ppm.Be specifically as follows 50ppm, 70ppm,
100ppm, 120ppm, 150ppm, 160ppm, 180ppm, 200ppm etc..
In an embodiment of the present invention, in step a), the additive amount of hydrocarbon solvent is the 5- of raw material acrylic resin quality
20 times, the additive amount of complexing agent is 3-15 times of raw material acrylic resin quality.Specifically, the additive amount of hydrocarbon solvent can be
The additive amount of 5 times, 8 times, 10 times, 12 times, 15 times, 18 times, 20 times etc. of raw material acrylic resin quality, complexing agent can be original
3 times, 5 times, 7 times, 10 times, 12 times, 15 times etc. for expecting acrylic resin quality.
It may be noted that raw material acrylic resin quality, that is, raw material to be processed acrylic resin herein.
In an embodiment of the present invention, in step b), the additive amount of hydrocarbon solvent is the 4- of raw material acrylic resin quality
16 times, the additive amount of complexing agent is 5-10 times of raw material acrylic resin quality, and the additive amount of alcohols solvent is raw material polypropylene
3-18 times of resin quality.Specifically, the additive amount of hydrocarbon solvent can be 4 times, 6 times, 8 of raw material acrylic resin quality
Again, 10 times, 13 times, 16 times etc., the additive amount of complexing agent can be 5 times, 6 times, 7 times, 8 times, 9 of raw material acrylic resin quality
Again, 10 times etc., the additive amount of alcohols solvent can be 3 times, 5 times, 7 times, 10 times, 12 times, 14 of raw material acrylic resin quality
Again, 16 times, 18 times etc..
In an embodiment of the present invention, in step c), the additive amount of complexing agent is 4-8 times of raw material acrylic resin, alcohol
The additive amount of class solvent is 5-15 times of raw material acrylic resin.Specifically, the additive amount of complexing agent can be raw material polypropylene
4 times, 5 times, 6 times, 7 times, 8 times etc. of resin, the additive amount of alcohols solvent can be 5 times, 7 times, 9 of raw material acrylic resin
Again, 12 times, 15 times etc..
In an embodiment of the present invention, in step d), the additive amount of alcohols solvent is 5-15 times of raw material acrylic resin.
Specifically, the additive amount of alcohols solvent is 5 times, 7 times, 9 times, 12 times, 15 times etc. of raw material acrylic resin.
May be noted that step a)-d) in, hydrocarbon solvent, complexing agent, alcohols solvent may be the same or different.
In an embodiment of the present invention, step a)-d) in, being warming up to temperature is 60-140 DEG C, and the time of stirring is 0.2-4
Hour；Preferably, step a)-d) in, being warming up to temperature is 60-100 DEG C, and the time of closed stirring is 1-3 hours.Specifically,
Being warming up to temperature can be 60 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, 120 DEG C, 140 DEG C etc..Wherein, closed stirring is using on washing kettle
Add reflux condensing tube to realize, prevents solvent from largely losing.
It in an embodiment of the present invention, further include step f): by final obtained solid resin drying materials, crushing, packaging
Obtain product.
Below in conjunction with embodiment, the present invention will be described in detail.
Embodiment 1A kind of production method of low ash component polypropylene resin, includes the following steps:
The content of ashes of raw material acrylic resin to be processed is 111.8ppm, isotacticity 95.3%；
A) once washing: above-mentioned raw materials polypropylene 1kg is added into washing kettle, by n-hexane 10kg and acetylacetone,2,4-pentanedione 5kg
The mixing lotion one of composition is warming up to 60 DEG C, washs 1.5h, is centrifugated, and discharging obtains hard resin material one；
B) secondary washing: step a) obtained solid resin material one is put into washing kettle, is added by n-hexane 8kg, second
The mixing lotion two of acyl acetone 7kg, ethyl alcohol 8kg composition, is warming up to 70 DEG C, washs 1h, be centrifugated, and discharging obtains hard resin
Material two；
C) it washs three times: step b) obtained solid resin material two is put into washing kettle, be added by acetylacetone,2,4-pentanedione 6kg,
The mixing lotion three of ethyl alcohol 10kg composition, is warming up to 80 DEG C, washs 2h, is centrifugated, and discharging obtains hard resin material three；
D) four washings: step c) obtained solid resin material three is put into washing kettle, and ethyl alcohol 10kg is added, is warming up to
80 DEG C, wash 1h, centrifuge separation, hard resin material four；
Then a step c)-d is answered to obtained solid resin material quadruple) after, by final step d) obtained solid resin
Product is packed to obtain in drying materials, crushing.
Embodiment 2A kind of production method of low ash component polypropylene resin, includes the following steps:
The content of ashes of raw material acrylic resin to be processed is 111.8ppm, isotacticity 95.3%；
A) once washing: above-mentioned raw materials polypropylene 1kg is added into washing kettle, by isooctane 5kg, acetylacetone,2,4-pentanedione 3kg group
At mixing lotion one, be warming up to 70 DEG C, wash 1h, be centrifugated, discharging obtains hard resin material one；
B) secondary washing: step a) obtained solid resin material one is put into washing kettle, is added by isooctane 4kg, second
The mixing lotion two of acyl acetone 5kg composition, ethyl alcohol 3kg are warming up to 80 DEG C, wash 1h, are centrifugated, and discharging obtains hard resin
Material two；
C) it washs three times: step b) obtained solid resin material two is put into washing kettle, be added by acetylacetone,2,4-pentanedione 4kg,
The mixing lotion three of ethyl alcohol 5kg composition, is warming up to 80 DEG C, washs 1h, is centrifugated, and discharging obtains hard resin material three；
D) four washings: step c) obtained solid resin material three is put into washing kettle, and ethyl alcohol 8kg is added, is warming up to
80 DEG C, wash 1h, centrifuge separation, hard resin material four；
Then a step c)-d is answered to obtained solid resin material quadruple) after, by final step d) obtained solid resin
Product is packed to obtain in drying materials, crushing.
Embodiment 3A kind of production method of low ash component polypropylene resin, includes the following steps:
The content of ashes of raw material acrylic resin to be processed is 111.8ppm, isotacticity 95.3%；
A) once washing: raw material polypropylene 1kg is added into washing kettle, by pentane 8kg, normal heptane 10g, acetylacetone,2,4-pentanedione
The mixing lotion one of 15kg composition, is warming up to 90 DEG C, washs 3h, is centrifugated, and discharging obtains hard resin material one；
B) secondary washing: step a) obtained solid resin material one is put into washing kettle, is added by pentane 16kg, acetyl
The mixing lotion two of acetone 10kg composition, isopropanol 18kg are warming up to 100 DEG C, wash 2h, are centrifugated, and discharging obtains solid tree
Rouge material two；
C) it washs three times: step b) obtained solid resin material two is put into washing kettle, be added by acetylacetone,2,4-pentanedione 8kg,
The mixing lotion three of isopropanol 15kg composition, is warming up to 110 DEG C, washs 1h, is centrifugated, and discharging obtains hard resin material three；
D) four washings: step c) obtained solid resin material three is put into washing kettle, and isopropanol 15kg, heating is added
To 120 DEG C, 1h is washed, is centrifugated, discharging obtains hard resin material four；
Then a step c)-d is answered to obtained solid resin material quadruple) after, by final step d) obtained solid resin
Product is packed to obtain in drying materials, crushing.
Embodiment 4With embodiment 1, the difference is that, mixing lotion one is n-decane 5kg, toluene 2kg, EDTA saturation
Solution 15kg；Mixing lotion two is n-decane 7kg, acetylacetone,2,4-pentanedione 8kg, amylalcohol 4kg, enanthol 4kg；Mixing lotion three is levulinic
Ketone 8kg, ethyl alcohol 10kg.
Embodiment 5With embodiment 1, the difference is that, acrylic resin raw material ash content to be processed is 51.8ppm, isotactic
Degree is 95.7%.
Embodiment 6With embodiment 1, the difference is that, acrylic resin raw material ash content to be processed is 194.6ppm, isotactic
Degree is 94.9%, repeats three times step c)-d).
Comparative example 1
With embodiment 1, the difference is that, omit step a) once washing.
Comparative example 2
With embodiment 1, the difference is that, omit step b) secondary washing.
Comparative example 3
With embodiment 1, the difference is that, it omits step c) and washs three times.
Comparative example 4
With embodiment 1, the difference is that, reverse step c) is washed three times and the sequence of step a) once washing.
Comparative example 5
Step a)-d) in be all made of ethyl alcohol as lotion.
Gained embodiment 1-6 and comparative example 1-5 products obtained therefrom are subjected to ash content test, specific as follows:
Acrylic resin is put into microwave dissolver, 6mL concentrated nitric acid and 2mL hydrogen peroxide is added clears up it completely and be
Clear solution is settled to 50mL later, carries out test sample analysis by icp ms, reference standard curve is surveyed
Determine each element content of ashes in digestion solution, calculated according to following formula:
In formula: W --- metal content of ashes in polypropylene, μ g/g (certain element quality/polypropylene quality)；ρ --- resolution
Concentration of element in liquid, μ g/ml；M --- weigh polyacrylic quality, g.It the results are shown in Table 1.
1 product acrylic resin total ashes of table and each element content
Gained embodiment 1-6 and comparative example 1-5 products obtained therefrom are subjected to isotacticity survey according to national standard GB/T2412-2008
Examination, concrete outcome are as follows:
2 product polypropylene resin isotactic degree of table
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of production method of low ash component polypropylene resin, including raw material acrylic resin to be processed is washed, it is special
Sign is that the washing includes the following steps:
A) once washing: raw material acrylic resin to be processed is put into washing kettle, and addition is made of hydrocarbon solvent and complexing agent
Mixing lotion one, after heating, closed stirring, centrifugal discharge obtains hard resin material one；
B) secondary washing: will step a) obtained solid resin material one put into washing kettle in, be added by hydrocarbon solvent, complexing agent and
The mixing lotion two of alcohols solvent composition, after heating, closed stirring, centrifugal discharge obtains hard resin material two；
C) it washs three times: step b) obtained solid resin material two is put into washing kettle, be added by complexing agent and alcohols solvent
The mixing lotion three of composition, after heating, closed stirring, centrifugal discharge obtains hard resin material three；
D) four washings: step c) obtained solid resin material three is put into washing kettle, and alcohols solvent is added, close after heating
Stirring is closed, centrifugal discharge obtains hard resin material four.
2. production method according to claim 1, which is characterized in that the content of ashes of final obtained solid resin material four
≤50ppm。
3. production method according to claim 2, which is characterized in that the method also includes step e): step d) terminates
Afterwards, step c)-d is repeated).
4. production method according to claim 1, which is characterized in that the hydrocarbon solvent includes in alkane and aromatic hydrocarbon
One or two kinds of mixing, wherein the carbon atom number of the alkane is 5-20；Preferably, the alkane includes pentane, isoamyl
The mixing of one or more of alkane, n-hexane, normal heptane, normal octane, isooctane, n -nonane, n-decane, the fragrance
Hydrocarbon includes the mixing of one or more of toluene, ethylbenzene, dimethylbenzene, trimethylbenzene；
The complexing agent includes acetylacetone,2,4-pentanedione, ethylenediamine tetra-acetic acid (EDTA), oxalic acid, tartaric acid, malonic acid, one in citric acid
Kind or two or more mixing；
The alcohols solvent includes methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, amylalcohol, hexanol, 2- methyl anyl alcohol, 2- ethyl fourth
The mixing of one or more of alcohol, enanthol, 2-Ethylhexyl Alcohol, octanol and decyl alcohol.
5. production method according to claim 1, which is characterized in that in step a), the additive amount of hydrocarbon solvent is raw material
5-20 times of acrylic resin quality, the additive amount of complexing agent are 3-15 times of raw material acrylic resin quality.
6. production method according to claim 1, which is characterized in that in step b), the additive amount of hydrocarbon solvent is raw material
4-16 times of acrylic resin quality, the additive amount of complexing agent are 5-10 times of raw material acrylic resin quality, alcohols solvent
Additive amount is 3-18 times of raw material acrylic resin quality.
7. production method according to claim 1, which is characterized in that in step c), the additive amount of complexing agent is poly- for raw material
4-8 times of allyl resin, the additive amount of alcohols solvent are 5-15 times of raw material acrylic resin.
8. production method according to claim 1, which is characterized in that in step d), the additive amount of alcohols solvent is raw material
5-15 times of acrylic resin.
9. production method according to claim 1, which is characterized in that step a)-d), being warming up to temperature is 60-140 DEG C,
The time of closed stirring is 0.2-4 hours；Preferably, being warming up to temperature is 60-100 DEG C, and the time of closed stirring is that 1-3 is small
When.
10. -9 described in any item production methods according to claim 1, which is characterized in that the method also includes step f): will
Product is dried, crushed, packing and to be obtained to final obtained solid resin material four.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113621096A (en) * | 2021-07-06 | 2021-11-09 | 雷剑兰 | Ultra-low ash polyolefin, preparation method and application |
| CN115124635A (en) * | 2022-07-29 | 2022-09-30 | 山东京博石油化工有限公司 | Deashing method of polyolefin material |
| CN115612005A (en) * | 2022-11-09 | 2023-01-17 | 山东京博石油化工有限公司 | Efficient solvent deashing treatment method for polypropylene resin |
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| CN115612005A (en) * | 2022-11-09 | 2023-01-17 | 山东京博石油化工有限公司 | Efficient solvent deashing treatment method for polypropylene resin |
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