CN106751876A - A kind of production method of high temperature resistant composite elasticizer - Google Patents
A kind of production method of high temperature resistant composite elasticizer Download PDFInfo
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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Abstract
The present invention is a kind of production method of high temperature resistant composite elasticizer, is comprised the following steps：(i) plasticizer matrix is prepared；(ii) flame-retardant system is prepared；(iii) high temperature resistant system is prepared；(iv) high temperature resistant composite elasticizer is prepared：Plasticizer matrix, flame-retardant system and high temperature resistant system obtained in above-mentioned steps are mixed in proportion, the addition of flame-retardant system is the 1.5 2.6% of plasticizer matrix weight, the addition of high temperature resistant system is the 3.2 3.5% of plasticizer matrix weight.The plasticizer feature of environmental protection of present invention production is good, and plasticizing efficiency is high, high temperature resistant, and volatility is low, volatility is extremely low, good stability, and with resistance to elevated temperatures, fire resistance, mechanical property, thermal stability and antistatic property.
Description
Technical field
The present invention relates to a kind of production method of plasticizer, specifically a kind of producer of high temperature resistant composite elasticizer
Method.
Background technology
Plasticizer is a kind of macromolecular material auxiliary agent, and its species is various, and most common kind is DEHP（Trade name
DOP）, DEHP chemical names phthalic acid two (2- ethyl hexyls) ester is a kind of colourless, liquid with no taste, is industrially widely used.Increase
Modeling agent is the industrial macromolecular material auxiliary agent being widely used, and this material is added in plastic processing, and its can be made flexible
Property enhancing, be easily worked, can be legal for industrial use.Domestic plasticizer is main based on conventional plasticizers at present, commonly
Plasticizer can only meet the requirement of common product, and non-environmental protection；The resistance to height such as electric wire for automobile, special cable, automotive trim instrument board
Warm plasticizer requirement is high, and existing common plasticizer cannot meet the requirement such as its low fogging, low volatilization, high temperature resistant.
The content of the invention
The technical problems to be solved by the invention are：
(1) how the fire-retardant and high-temperature resistant result of plasticizer is improved by adding fire retardant and high temperature resistant agent；
(2) cause the plastics mechanical property by the plasticizer production low after how improving due to adding fire retardant and high temperature resistant agent
Technical problem.
The present invention solve above technical problem technical scheme be：
A kind of production method of high temperature resistant composite elasticizer, comprises the following steps：
(i) plasticizer matrix is prepared：
(1) it is esterified：The C8-10 fatty alcohols that will be measured by proportioning squeeze into reactor, and temperature of reaction kettle is added after being less than 80 DEG C by proportioning
Enter trimellitic anhydride, then add catalyst by proportioning again, when material temperature rises to 220-225 DEG C, start negative reaction, work as acid number
＜ 0.1mgKOH/g, carry out flash distillation dealcoholysis；The weight of trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic anhydride：1
Part, C8-10 fatty alcohols：2.2-3.0 parts；The addition of catalyst is the 0.1- of trimellitic anhydride and C8-10 fatty alcohol gross weights
1%；
(2) refine：Flash distillation adds sodium carbonate to be neutralized after terminating by proportioning, neutralizes time 10-25 minute, temperature of reaction kettle liter
During to 220-225 DEG C, start stripping, after then material temperature is down to 210-215 DEG C from 220-225 DEG C, keep 210-215 DEG C of stripping
2.5-3h, and cooling down after being incubated half an hour, and add the auxiliary material to carry out refined stirring by proportioning；The addition of sodium carbonate is inclined benzene three
The 0.1-0.7% of acid anhydrides and C8-10 fatty alcohol gross weights, the addition of auxiliary material is trimellitic anhydride and C8-10 fatty alcohol gross weights
0.3-1%；
(3) press filtration is refined：Regulation filter pump bypass valve filter internal pressure power is maintained at 0.3~0.5Mpa, treat press filtration material without and
When pressure declines in filter, terminate press filtration；
(4) distill：The vacuum system of molecular distillation equipment is opened, vavuum pump is run so that the vacuum of molecular distillation equipment system
Reach within 100pa, open heat conduction oil circulating pump, the material inlet temperature of molecular distillation equipment system is maintained at 218 ± 5
DEG C, the bottom valve of finished pot and the sample introduction valve of molecular distillation equipment system are opened, sample introduction 20 ± 5HZ of frequency is kept, enter
Sample flow 0.6m3-1m3, the separation reductor of molecular distillation equipment is opened, frequency is kept stirring for for 45 ± 5HZ, product is in molecule
Purification weight component is automatically separated in distillation equipment, heavy constituent finished product is collected, finished pot storage is transferred to；
(ii) flame-retardant system is prepared：By nano silicon, ethoxylated alkylamine, Methyl Hydrogen Polysiloxane Fluid, hydroxyl poly dimethyl silicon
Oxygen alkane, vinyltrimethoxy silane, APP, reactive diluent, compatilizer, coupling agent, levelling agent and mixed chlorinated dilute
Soil is mixed in proportion, and specific weight is：Nano silicon：2.7-2.9 parts, ethoxylated alkylamine：25-27
Part, Methyl Hydrogen Polysiloxane Fluid：41-43 parts, hydroxyl dimethyl silicone polymer：6.7-6.9 parts, vinyltrimethoxy silane：5.8-6
Part, APP：4.5-4.7 parts, reactive diluent：1.5-1.7 parts, compatilizer：2.5-2.7 parts, coupling agent：1.1-1.3 parts,
Levelling agent：0.5-0.7 parts, mixed chlorinated rare earth：0.3-0.5 parts；The particle diameter of described nano silicon is 20-30nm；
(iii) high temperature resistant system is prepared：By nano imvite, fume colloidal silica, nano zine oxide, gamma-aminopropyl-triethoxy silicon
Alkane, APES and mixed chlorinated rare earth are mixed in proportion；Specifically weight is：Nano imvite：
12-15 parts, fume colloidal silica：5.5-5.7 parts, nano zine oxide：2.5-2.7 parts, gamma-aminopropyl-triethoxy-silane：22-
25 parts, APES：5.1-5.3 parts, mixed chlorinated rare earth：0.3-0.5 parts；The particle diameter of described nano imvite
It is 20-30nm；
(iv) high temperature resistant composite elasticizer is prepared：Plasticizer matrix, flame-retardant system and high temperature resistant system obtained in above-mentioned steps are pressed
Ratio is well mixed, and the addition of flame-retardant system is the 1.5-2.6% of plasticizer matrix weight, and the addition of high temperature resistant system is
The 3.2-3.5% of plasticizer matrix weight.
The technical scheme that further limits of the invention is：
The production method of foregoing high temperature resistant composite elasticizer, wherein catalyst are for isopropyl titanate, tetrabutyl titanate and to first
One or more mixing in benzene sulfonic acid；Auxiliary material is diatomite or activated carbon.
The production method of foregoing high temperature resistant composite elasticizer, wherein reactive diluent are alkyl glycidyl ether, Xin Kui
In acid glycidyl ester, trihydroxymethylpropanyltri diglycidyl ether, toluene glycidol ether, castor oil polyglycidyl ether one
Plant or more than one mixtures；The compatilizer is maleic anhydride grafted PP；Coupling agent is the diacetylmonoxime of vinyl three
One kind or one kind in base silane coupling agent, methylvinyldichlorosilane coupling agent, methyl tributanoximo silane coupling agent
Thing mixed above；Levelling agent is isophorone, DAA, fluorin modified crylic acid, phosphate modified acrylic acid, acrylic acid, poly-
One or more mixtures in dimethyl siloxane, poly- methyl alkyl siloxane, organic modified polyorganosiloxane.
The beneficial effects of the invention are as follows：Experimental result shows that flame-retardant system of the invention can be effectively improved the resistance of plasticizer
Combustion performance, when nano silicon, ethoxylated alkylamine, Methyl Hydrogen Polysiloxane Fluid, hydroxyl dimethyl silicone polymer, vinyl three
After methoxy silane and APP composition flame-retardant system add plasticizer matrix, limited oxygen index lifting 22% or so can be made, and
There is coordinative role in the addition of reactive diluent, compatilizer, coupling agent, levelling agent and mixed chlorinated rare earth, can be significantly further
The fire resistance of lifting plasticizer of the present invention, makes limited oxygen index further be promoted to 31% or so.Observed by SEM and found, received
Rice silica, ethoxylated alkylamine, Methyl Hydrogen Polysiloxane Fluid, hydroxyl dimethyl silicone polymer, vinyltrimethoxy silane
With APP constitute flame-retardant system in plasticizer matrix dispersiveness it is poor, add reactive diluent, compatilizer, coupling agent,
The dispersiveness of flame-retardant system can be improved after levelling agent and mixed chlorinated rare earth.In addition, in electric wire for automobile and automotive trim instrument
After high temperature resistant composite elasticizer of the invention is added in disk plastic processing, because the addition of flame-retardant system can make the mechanical property of plastics
Can make it compared to having declined, but after with the addition of reactive diluent, compatilizer, coupling agent, levelling agent and mixed chlorinated rare earth
Mechanical property makes moderate progress, and can meet or exceed the mechanical requirements of itself.Synthesis result shows, when the addition of flame-retardant system
It is the 1.5-2.6% of plasticizer matrix weight to measure, and the limited oxygen index of plasticizer has reached 31.2%, and flame retarding efficiency is high, its resistance
Combustion performance, three kinds of performances of mechanical property and heat endurance reach an equalization point, fire resistance, mechanical property and thermally-stabilised
Property is more excellent.In addition, experimental result shows, the addition of high temperature resistant system of the present invention can be effectively improved the heat-resisting quantity of plasticizer
Can, the addition of same exotic material nano imvite, fume colloidal silica and nano zine oxide can make plasticizer of the present invention
Mechanical property has declined, but with the addition of gamma-aminopropyl-triethoxy-silane, APES and mixed chlorinated rare earth
Their mechanical property can be made to make moderate progress afterwards；Find to add gamma-aminopropyl-triethoxy-silane, alkyl phenol by ESEM
The compatibility of exotic material and plasticizer matrix can be improved after APEO and mixed chlorinated rare earth.Synthesis result shows
Show, when the addition of high temperature resistant system is the 3.2-3.5% of plasticizer matrix weight, its resistance to elevated temperatures, fire resistance, mechanics
Four kinds of performances of performance and heat endurance reach an equalization point, and various performances are more excellent.In addition, flame-retardant system of the present invention plus
Enter the antistatic performance that can also effectively improve plasticizer, obtain unexpected technique effect.In sum, the present invention passes through
Flame-retardant system and high temperature resistant system are added, the resistance to elevated temperatures of plasticizer, fire resistance, mechanical property, thermally-stabilised can be improved
Performance and antistatic property；And the plasticizer matrix feature of environmental protection is good obtained in production method of the present invention, plasticizing efficiency is high, resistance to height
Temperature, volatility is low, volatility is extremely low, good stability.The degree of atomization of plasticizer matrix of the invention and existing plasticizer is to such as
Under：DOP：4.9mg, DPHP：1.0mg, DIDP：0.8mg, TOTM：0.2mg, plasticizer matrix of the present invention：0.1 mg.
Specific embodiment
Embodiment 1
The present embodiment is a kind of production method of high temperature resistant composite elasticizer, is comprised the following steps：
(i) plasticizer matrix is prepared：
(1) it is esterified：The C8-10 fatty alcohols that will be measured by proportioning squeeze into reactor, and temperature of reaction kettle is added after being less than 80 DEG C by proportioning
Enter trimellitic anhydride, then add catalyst by proportioning again, when material temperature rises to 220 DEG C, start negative reaction, as acid number ＜
0.1mgKOH/g, carries out flash distillation dealcoholysis；The weight of trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic anhydride：1 part,
C8-10 fatty alcohols：2.2 parts；The addition of catalyst is the 0.1% of trimellitic anhydride and C8-10 fatty alcohol gross weights；Wherein urge
Agent is one or more mixing in isopropyl titanate, tetrabutyl titanate and p-methyl benzenesulfonic acid；
(2) refine：Flash distillation adds sodium carbonate to be neutralized after terminating by proportioning, neutralizes 10 minutes time, and temperature of reaction kettle rises to
At 220 DEG C, start stripping, after then material temperature is down to 210 DEG C from 220 DEG C, keep 210 DEG C of stripping 2.5h, and after being incubated half an hour
Cooling, and carry out refined stirring by proportioning addition auxiliary material；The addition of sodium carbonate is trimellitic anhydride and C8-10 fatty alcohol gross weights
The 0.1% of amount, the addition of auxiliary material is the 0.3% of trimellitic anhydride and C8-10 fatty alcohol gross weights；Auxiliary material is diatomite or work
Property charcoal；
(3) press filtration is refined：Regulation filter pump bypass valve makes filter internal pressure power be maintained at 0.3Mpa, treats that press filtration material is no and filters
When pressure declines in machine, terminate press filtration；
(4) distill：The vacuum system of molecular distillation equipment is opened, vavuum pump is run so that the vacuum of molecular distillation equipment system
Reach within 100pa, open heat conduction oil circulating pump, the material inlet temperature of molecular distillation equipment system is maintained at 213 DEG C, beat
The bottom valve of finished pot and the sample introduction valve of molecular distillation equipment system are opened, sample introduction frequency 15HZ, sample introduction flow is kept
0.6m3, open the separation reductor of molecular distillation equipment, be kept stirring for frequency for 40HZ, product in molecular distillation equipment from
Dynamic separating-purifying weight component, collects heavy constituent finished product, is transferred to finished pot storage；
(ii) flame-retardant system is prepared：By nano silicon, ethoxylated alkylamine, Methyl Hydrogen Polysiloxane Fluid, hydroxyl poly dimethyl silicon
Oxygen alkane, vinyltrimethoxy silane, APP, reactive diluent, compatilizer, coupling agent, levelling agent and mixed chlorinated dilute
Soil is mixed in proportion；The component of the weight portion of flame-retardant system is configured to：Nano silicon：2.7 parts, ethoxylated alkyl
Amine：25 parts, Methyl Hydrogen Polysiloxane Fluid：41 parts, hydroxyl dimethyl silicone polymer：6.7 parts, vinyltrimethoxy silane：5.8 parts,
APP：4.5 parts, reactive diluent：1.5 parts, compatilizer：2.5 parts, coupling agent：1.1 parts, levelling agent：0.5 part, mix chlorine
Change rare earth：0.3 part；The particle diameter of nano silicon is 20nm；Reactive diluent is alkyl glycidyl ether, pungent certain herbaceous plants with big flowers is sour shrinks sweet
One kind or one kind in grease, trihydroxymethylpropanyltri diglycidyl ether, toluene glycidol ether, castor oil polyglycidyl ether
Thing mixed above；Compatilizer is maleic anhydride grafted PP；Coupling agent be vinyl tributyl ketoximyl silane coupling agent,
One or more mixtures in methylvinyldichlorosilane coupling agent, methyl tributanoximo silane coupling agent；Stream
Flat agent be isophorone, DAA, fluorin modified crylic acid, phosphate modified acrylic acid, acrylic acid, dimethyl silicone polymer,
One or more mixtures in poly- methyl alkyl siloxane, organic modified polyorganosiloxane；
(iii) high temperature resistant system is prepared：By nano imvite, fume colloidal silica, nano zine oxide, gamma-aminopropyl-triethoxy silicon
Alkane, APES and mixed chlorinated rare earth are mixed in proportion；The component of the weight portion of high temperature resistant system is constituted
For：Nano imvite：12 parts, fume colloidal silica：5.5 parts, nano zine oxide：2.5 parts, gamma-aminopropyl-triethoxy-silane：
22 parts, APES：5.1 parts, mixed chlorinated rare earth：0.3 part；The particle diameter of nano imvite is 20nm；
(iv) high temperature resistant composite elasticizer is prepared：Plasticizer matrix, flame-retardant system and high temperature resistant system obtained in above-mentioned steps are pressed
Ratio is well mixed, and the addition of flame-retardant system is the 1.5% of plasticizer matrix weight, and the addition of high temperature resistant system is plasticising
The 3.2% of agent matrix weight.
Embodiment 2
The present embodiment is a kind of production method of high temperature resistant composite elasticizer, is comprised the following steps：
(i) plasticizer matrix is prepared：
(1) it is esterified：The C8-10 fatty alcohols that will be measured by proportioning squeeze into reactor, and temperature of reaction kettle is added after being less than 80 DEG C by proportioning
Enter trimellitic anhydride, then add catalyst by proportioning again, when material temperature rises to 223 DEG C, start negative reaction, as acid number ＜
0.1mgKOH/g, carries out flash distillation dealcoholysis；The weight of trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic anhydride：1 part,
C8-10 fatty alcohols：2.6 parts, the addition of catalyst is the 0.5% of trimellitic anhydride and C8-10 fatty alcohol gross weights；Catalyst
It is one or more mixing in isopropyl titanate, tetrabutyl titanate and p-methyl benzenesulfonic acid；
(2) refine：Flash distillation adds sodium carbonate to be neutralized after terminating by proportioning, neutralizes 20 minutes time, and temperature of reaction kettle rises to
At 223 DEG C, start stripping, after then material temperature is down to 212 DEG C from 223 DEG C, keep 212 DEG C of stripping 2.8h, and after being incubated half an hour
Cooling, and carry out refined stirring by proportioning addition auxiliary material；The addition of sodium carbonate is trimellitic anhydride and C8-10 fatty alcohol gross weights
The 0.3% of amount, the addition of auxiliary material is the 0.6% of trimellitic anhydride and C8-10 fatty alcohol gross weights；Auxiliary material is diatomite or work
Property charcoal；
(3) press filtration is refined：Regulation filter pump bypass valve makes filter internal pressure power be maintained at 0.4Mpa, treats that press filtration material is no and filters
When pressure declines in machine, terminate press filtration；
(4) distill：The vacuum system of molecular distillation equipment is opened, vavuum pump is run so that the vacuum of molecular distillation equipment system
Reach within 100pa, open heat conduction oil circulating pump, the material inlet temperature of molecular distillation equipment system is maintained at 218 DEG C, beat
The bottom valve of finished pot and the sample introduction valve of molecular distillation equipment system are opened, sample introduction frequency 20HZ, sample introduction flow is kept
0.8m3, open the separation reductor of molecular distillation equipment, be kept stirring for frequency for 45HZ, product in molecular distillation equipment from
Dynamic separating-purifying weight component, collects heavy constituent finished product, is transferred to finished pot storage；
(ii) flame-retardant system is prepared：By nano silicon, ethoxylated alkylamine, Methyl Hydrogen Polysiloxane Fluid, hydroxyl poly dimethyl silicon
Oxygen alkane, vinyltrimethoxy silane, APP, reactive diluent, compatilizer, coupling agent, levelling agent and mixed chlorinated dilute
Soil is mixed in proportion；The component of the weight portion of flame-retardant system is configured to：Nano silicon：2.8 parts, ethoxylated alkyl
Amine：26 parts, Methyl Hydrogen Polysiloxane Fluid：42 parts, hydroxyl dimethyl silicone polymer：6.8 parts, vinyltrimethoxy silane：5.9 parts,
APP：4.6 parts, reactive diluent：1.6 parts, compatilizer：2.6 parts, coupling agent：1.2 parts, levelling agent：0.6 part, mix chlorine
Change rare earth：0.4 part；The particle diameter of nano silicon is 25nm；Reactive diluent is alkyl glycidyl ether, pungent certain herbaceous plants with big flowers is sour shrinks sweet
One kind or one kind in grease, trihydroxymethylpropanyltri diglycidyl ether, toluene glycidol ether, castor oil polyglycidyl ether
Thing mixed above；The compatilizer is maleic anhydride grafted PP；Coupling agent is vinyl tributyl ketoximyl silane idol
One or more mixing in connection agent, methylvinyldichlorosilane coupling agent, methyl tributanoximo silane coupling agent
Thing；Levelling agent is isophorone, DAA, fluorin modified crylic acid, phosphate modified acrylic acid, acrylic acid, poly dimethyl silicon
One or more mixtures in oxygen alkane, poly- methyl alkyl siloxane, organic modified polyorganosiloxane；
(iii) high temperature resistant system is prepared：By nano imvite, fume colloidal silica, nano zine oxide, gamma-aminopropyl-triethoxy silicon
Alkane, APES and mixed chlorinated rare earth are mixed in proportion；The component of the weight portion of high temperature resistant system is constituted
For：Nano imvite：13 parts, fume colloidal silica：5.6 parts, nano zine oxide：2.6 parts, gamma-aminopropyl-triethoxy-silane：
23 parts, APES：5.2 parts, mixed chlorinated rare earth：0.4 part；The particle diameter of nano imvite is 25nm；
(iv) high temperature resistant composite elasticizer is prepared：Plasticizer matrix, flame-retardant system and high temperature resistant system obtained in above-mentioned steps are pressed
Ratio is well mixed, and the addition of flame-retardant system is the 2.0% of plasticizer matrix weight, and the addition of high temperature resistant system is plasticising
The 3.3% of agent matrix weight.
Embodiment 3
The present embodiment is a kind of production method of high temperature resistant composite elasticizer, is comprised the following steps：
(i) plasticizer matrix is prepared：
(1) it is esterified：The C8-10 fatty alcohols that will be measured by proportioning squeeze into reactor, and temperature of reaction kettle is added after being less than 80 DEG C by proportioning
Enter trimellitic anhydride, then add catalyst by proportioning again, when material temperature rises to 225 DEG C, start negative reaction, as acid number ＜
0.1mgKOH/g, carries out flash distillation dealcoholysis；The weight of trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic anhydride：1 part,
C8-10 fatty alcohols：3.0 parts, the addition of catalyst is the 1% of trimellitic anhydride and C8-10 fatty alcohol gross weights；Catalyst is
One or more mixing in isopropyl titanate, tetrabutyl titanate and p-methyl benzenesulfonic acid；
(2) refine：Flash distillation adds sodium carbonate to be neutralized after terminating by proportioning, neutralizes 25 minutes time, and temperature of reaction kettle rises to
At 225 DEG C, start stripping, after then material temperature is down to 215 DEG C from 225 DEG C, keep 215 DEG C of stripping 2.5-3h, and be incubated half an hour
After cool down, and add the auxiliary material to carry out refined stirring by proportioning；The addition of sodium carbonate is that trimellitic anhydride and C8-10 fatty alcohols are total
The 0.7% of weight, the addition of auxiliary material is the 1% of trimellitic anhydride and C8-10 fatty alcohol gross weights；Auxiliary material is diatomite or work
Property charcoal；
(3) press filtration is refined：Regulation filter pump bypass valve makes filter internal pressure power be maintained at 0.5Mpa, treats that press filtration material is no and filters
When pressure declines in machine, terminate press filtration；
(4) distill：The vacuum system of molecular distillation equipment is opened, vavuum pump is run so that the vacuum of molecular distillation equipment system
Reach within 100pa, open heat conduction oil circulating pump, the material inlet temperature of molecular distillation equipment system is maintained at 222 DEG C, beat
The bottom valve of finished pot and the sample introduction valve of molecular distillation equipment system are opened, sample introduction frequency 25HZ, sample introduction flow is kept
1m3, the separation reductor of molecular distillation equipment is opened, frequency is kept stirring for for 50HZ, product is automatic in molecular distillation equipment
Separating-purifying weight component, collects heavy constituent finished product, is transferred to finished pot storage；
(ii) flame-retardant system is prepared：By nano silicon, ethoxylated alkylamine, Methyl Hydrogen Polysiloxane Fluid, hydroxyl poly dimethyl silicon
Oxygen alkane, vinyltrimethoxy silane, APP, reactive diluent, compatilizer, coupling agent, levelling agent and mixed chlorinated dilute
Soil is mixed in proportion；The component of the weight portion of flame-retardant system is configured to：Nano silicon：2.9 parts, ethoxylated alkyl
Amine：27 parts, Methyl Hydrogen Polysiloxane Fluid：43 parts, hydroxyl dimethyl silicone polymer：6.9 parts, vinyltrimethoxy silane：6 parts, gather
Ammonium phosphate：4.7 parts, reactive diluent：1.7 parts, compatilizer：2.7 parts, coupling agent：1.3 parts, levelling agent：It is 0.7 part, mixed chlorinated
Rare earth：0.5 part；The particle diameter of nano silicon is 30nm；Reactive diluent is alkyl glycidyl ether, pungent certain herbaceous plants with big flowers acid glycidyl
One kind or one kind in ester, trihydroxymethylpropanyltri diglycidyl ether, toluene glycidol ether, castor oil polyglycidyl ether with
Upper mixture；The compatilizer is maleic anhydride grafted PP；Coupling agent is coupled for vinyl tributyl ketoximyl silane
One or more mixtures in agent, methylvinyldichlorosilane coupling agent, methyl tributanoximo silane coupling agent；
Levelling agent is isophorone, DAA, fluorin modified crylic acid, phosphate modified acrylic acid, acrylic acid, polydimethylsiloxanes
One or more mixtures in alkane, poly- methyl alkyl siloxane, organic modified polyorganosiloxane；
(iii) high temperature resistant system is prepared：By nano imvite, fume colloidal silica, nano zine oxide, gamma-aminopropyl-triethoxy silicon
Alkane, APES and mixed chlorinated rare earth are mixed in proportion；The component of the weight portion of high temperature resistant system is constituted
For：Nano imvite：15 parts, fume colloidal silica：5.7 parts, nano zine oxide：2.7 parts, gamma-aminopropyl-triethoxy-silane：
25 parts, APES：5.3 parts, mixed chlorinated rare earth：0.5 part；The particle diameter of nano imvite is 30nm；
(iv) high temperature resistant composite elasticizer is prepared：Plasticizer matrix, flame-retardant system and high temperature resistant system obtained in above-mentioned steps are pressed
Ratio is well mixed, and the addition of flame-retardant system is the 2.6% of plasticizer matrix weight, and the addition of high temperature resistant system is plasticising
The 3.5% of agent matrix weight.
In addition to the implementation, the present invention can also have other embodiment.All use equivalents or equivalent transformation shape
Into technical scheme, all fall within the protection domain of application claims.
Claims (6)
1. a kind of production method of high temperature resistant composite elasticizer, it is characterised in that：Comprise the following steps：
(i) plasticizer matrix is prepared：
(1) it is esterified：The C8-10 fatty alcohols that will be measured by proportioning squeeze into reactor, and temperature of reaction kettle is added after being less than 80 DEG C by proportioning
Enter trimellitic anhydride, then add catalyst by proportioning again, when material temperature rises to 220-225 DEG C, start negative reaction, work as acid number
＜ 0.1mgKOH/g, carry out flash distillation dealcoholysis；The weight of the trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic acid
Acid anhydride：1 part, C8-10 fatty alcohols：2.2-3.0 parts；The addition of the catalyst is trimellitic anhydride and C8-10 fatty alcohol gross weights
The 0.1-1% of amount；
(2) refine：Flash distillation adds sodium carbonate to be neutralized after terminating by proportioning, neutralizes time 10-25 minute, temperature of reaction kettle liter
During to 220-225 DEG C, start stripping, after then material temperature is down to 210-215 DEG C from 220-225 DEG C, keep 210-215 DEG C of stripping
2.5-3h, and cooling down after being incubated half an hour, and add the auxiliary material to carry out refined stirring by proportioning；The addition of the sodium carbonate is inclined
The 0.1-0.7% of benzenetricarboxylic anhydride and C8-10 fatty alcohol gross weights, the addition of the auxiliary material is trimellitic anhydride and C8-10 fat
The 0.3-1% of alcohol gross weight；
(3) press filtration is refined：Regulation filter pump bypass valve filter internal pressure power is maintained at 0.3~0.5Mpa, treat press filtration material without and
When pressure declines in filter, terminate press filtration；
(4) distill：The vacuum system of molecular distillation equipment is opened, vavuum pump is run so that the vacuum of molecular distillation equipment system
Reach within 100pa, open heat conduction oil circulating pump, the material inlet temperature of molecular distillation equipment system is maintained at 218 ± 5
DEG C, the bottom valve of finished pot and the sample introduction valve of molecular distillation equipment system are opened, sample introduction 20 ± 5HZ of frequency is kept, enter
Sample flow 0.6m3-1m3, the separation reductor of molecular distillation equipment is opened, frequency is kept stirring for for 45 ± 5HZ, product is in molecule
Purification weight component is automatically separated in distillation equipment, heavy constituent finished product is collected, finished pot storage is transferred to；
(ii) flame-retardant system is prepared：By nano silicon, ethoxylated alkylamine, Methyl Hydrogen Polysiloxane Fluid, hydroxyl poly dimethyl silicon
Oxygen alkane, vinyltrimethoxy silane, APP, reactive diluent, compatilizer, coupling agent, levelling agent and mixed chlorinated dilute
Soil is mixed in proportion, and specific weight is：Nano silicon：2.7-2.9 parts, ethoxylated alkylamine：25-27
Part, Methyl Hydrogen Polysiloxane Fluid：41-43 parts, hydroxyl dimethyl silicone polymer：6.7-6.9 parts, vinyltrimethoxy silane：5.8-6
Part, APP：4.5-4.7 parts, reactive diluent：1.5-1.7 parts, compatilizer：2.5-2.7 parts, coupling agent：1.1-1.3 parts,
Levelling agent：0.5-0.7 parts, mixed chlorinated rare earth：0.3-0.5 parts；The particle diameter of described nano silicon is 20-30nm；
(iii) high temperature resistant system is prepared：By nano imvite, fume colloidal silica, nano zine oxide, gamma-aminopropyl-triethoxy silicon
Alkane, APES and mixed chlorinated rare earth are mixed in proportion；Specifically weight is：Nano imvite：
12-15 parts, fume colloidal silica：5.5-5.7 parts, nano zine oxide：2.5-2.7 parts, gamma-aminopropyl-triethoxy-silane：22-
25 parts, APES：5.1-5.3 parts, mixed chlorinated rare earth：0.3-0.5 parts；The particle diameter of described nano imvite
It is 20-30nm；
(iv) high temperature resistant composite elasticizer is prepared：Plasticizer matrix, flame-retardant system and high temperature resistant system obtained in above-mentioned steps are pressed
Ratio is well mixed, and the addition of the flame-retardant system is the 1.5-2.6% of the plasticizer matrix weight, the high temperature resistant body
The addition of system is the 3.2-3.5% of the plasticizer matrix weight.
2. the production method of high temperature resistant composite elasticizer as claimed in claim 1, it is characterised in that：The catalyst is metatitanic acid
One or more mixing in isopropyl ester, tetrabutyl titanate and p-methyl benzenesulfonic acid；The auxiliary material is diatomite or activated carbon.
3. the production method of high temperature resistant composite elasticizer as claimed in claim 1, it is characterised in that：The reactive diluent is
Alkyl glycidyl ether, pungent certain herbaceous plants with big flowers acid glycidyl ester, trihydroxymethylpropanyltri diglycidyl ether, toluene glycidol ether, castor-oil plant
One or more mixtures in oily polyglycidyl ether；The compatilizer is maleic anhydride grafted PP；Institute
Coupling agent is stated for vinyl tributyl ketoximyl silane coupling agent, methylvinyldichlorosilane coupling agent, methyl tributanoximo
One or more mixtures in silane coupler；The levelling agent is isophorone, DAA, fluorine richness propylene
In sour, phosphate modified acrylic acid, acrylic acid, dimethyl silicone polymer, poly- methyl alkyl siloxane, organic modified polyorganosiloxane
One or more mixtures.
4. the production method of the high temperature resistant composite elasticizer as described in claim 1-3 any claims, it is characterised in that：Institute
The weight for stating trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic anhydride：1 part, C8-10 fatty alcohols：2.2 parts；It is described
The addition of catalyst is the 0.1% of trimellitic anhydride and C8-10 fatty alcohol gross weights, and the addition of the sodium carbonate is inclined benzene
The 0.1% of three acid anhydrides and C8-10 fatty alcohol gross weights, the addition of the auxiliary material is trimellitic anhydride and C8-10 fatty alcohol gross weights
The 0.3% of amount；The high temperature resistant composite elasticizer also includes flame-retardant system and high temperature resistant system, the addition of the flame-retardant system
It is the 1.5% of the plasticizer matrix weight, the addition of the high temperature resistant system is the 3.2% of the plasticizer matrix weight；
The component of the weight portion of the flame-retardant system is configured to：Nano silicon：2.7 parts, ethoxylated alkylamine：25 parts, methyl
Containing hydrogen silicone oil：41 parts, hydroxyl dimethyl silicone polymer：6.7 parts, vinyltrimethoxy silane：5.8 parts, APP：4.5
Part, reactive diluent：1.5 parts, compatilizer：2.5 parts, coupling agent：1.1 parts, levelling agent：0.5 part, mixed chlorinated rare earth：0.3
Part；The particle diameter of described nano silicon is 20nm；The component of the weight portion of the high temperature resistant system is configured to：Nanometer is covered de-
Soil：12 parts, fume colloidal silica：5.5 parts, nano zine oxide：2.5 parts, gamma-aminopropyl-triethoxy-silane：22 parts, alkyl phenol
APEO：5.1 parts, mixed chlorinated rare earth：0.3 part；The particle diameter of described nano imvite is 20nm.
5. the production method of the high temperature resistant composite elasticizer as described in claim 1-3 any claims, it is characterised in that：Institute
The weight for stating trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic anhydride：1 part, C8-10 fatty alcohols：2.6 parts；It is described
The addition of catalyst is the 0.5% of trimellitic anhydride and C8-10 fatty alcohol gross weights, and the addition of the sodium carbonate is inclined benzene
The 0.3% of three acid anhydrides and C8-10 fatty alcohol gross weights, the addition of the auxiliary material is trimellitic anhydride and C8-10 fatty alcohol gross weights
The 0.6% of amount；The high temperature resistant composite elasticizer also includes flame-retardant system and high temperature resistant system, the addition of the flame-retardant system
It is the 2.0% of the plasticizer matrix weight, the addition of the high temperature resistant system is the 3.3% of the plasticizer matrix weight；
The component of the weight portion of the flame-retardant system is configured to：Nano silicon：2.8 parts, ethoxylated alkylamine：26 parts, methyl
Containing hydrogen silicone oil：42 parts, hydroxyl dimethyl silicone polymer：6.8 parts, vinyltrimethoxy silane：5.9 parts, APP：4.6
Part, reactive diluent：1.6 parts, compatilizer：2.6 parts, coupling agent：1.2 parts, levelling agent：0.6 part, mixed chlorinated rare earth：0.4
Part；The particle diameter of described nano silicon is 25nm；The component of the weight portion of the high temperature resistant system is configured to：Nanometer is covered de-
Soil：13 parts, fume colloidal silica：5.6 parts, nano zine oxide：2.6 parts, gamma-aminopropyl-triethoxy-silane：23 parts, alkyl phenol
APEO：5.2 parts, mixed chlorinated rare earth：0.4 part；The particle diameter of described nano imvite is 25nm.
6. the production method of the high temperature resistant composite elasticizer as described in claim 1-3 any claims, it is characterised in that：Institute
The weight for stating trimellitic anhydride and C8-10 fatty alcohols is：Trimellitic anhydride：1 part, C8-10 fatty alcohols：3.0 parts；It is described
The addition of catalyst is the 1% of trimellitic anhydride and C8-10 fatty alcohol gross weights, and the addition of the sodium carbonate is inclined benzene three
The 0.7% of acid anhydrides and C8-10 fatty alcohol gross weights, the addition of the auxiliary material is trimellitic anhydride and C8-10 fatty alcohol gross weights
1%；The high temperature resistant composite elasticizer also includes flame-retardant system and high temperature resistant system, and the addition of the flame-retardant system is institute
The 2.6% of plasticizer matrix weight is stated, the addition of the high temperature resistant system is the 3.5% of the plasticizer matrix weight；It is described
The component of the weight portion of flame-retardant system is configured to：Nano silicon：2.9 parts, ethoxylated alkylamine：27 parts, methyl hydrogen
Silicone oil：43 parts, hydroxyl dimethyl silicone polymer：6.9 parts, vinyltrimethoxy silane：6 parts, APP：4.7 parts, activity
Diluent：1.7 parts, compatilizer：2.7 parts, coupling agent：1.3 parts, levelling agent：0.7 part, mixed chlorinated rare earth：0.5 part；Described
The particle diameter of nano silicon is 30nm；The component of the weight portion of the high temperature resistant system is configured to：Nano imvite：15 parts,
Fume colloidal silica：5.7 parts, nano zine oxide：2.7 parts, gamma-aminopropyl-triethoxy-silane：25 parts, alkylphenol-polyethenoxy
Ether：5.3 parts, mixed chlorinated rare earth：0.5 part；The particle diameter of described nano imvite is 30nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218700A (en) * | 2018-01-26 | 2018-06-29 | 江苏森禾化工科技有限公司 | A kind of automotive upholstery specialty plasticiser TM8 |
| CN114805928A (en) * | 2022-03-10 | 2022-07-29 | 江苏森禾化工科技有限公司 | Metabenzene bio-based plasticizer |
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| CN101973884A (en) * | 2010-09-26 | 2011-02-16 | 昆山合峰化工有限公司 | Method for preparing triisononyl trimellitate (TINTM) |
| CN103012150A (en) * | 2012-12-27 | 2013-04-03 | 江南大学 | Method for preparing plasticizer 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester |
| CN105237401A (en) * | 2015-10-16 | 2016-01-13 | 江苏森禾化工科技有限公司 | Manufacturing technology of plasticizer |
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| CN101973884A (en) * | 2010-09-26 | 2011-02-16 | 昆山合峰化工有限公司 | Method for preparing triisononyl trimellitate (TINTM) |
| CN103012150A (en) * | 2012-12-27 | 2013-04-03 | 江南大学 | Method for preparing plasticizer 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108218700A (en) * | 2018-01-26 | 2018-06-29 | 江苏森禾化工科技有限公司 | A kind of automotive upholstery specialty plasticiser TM8 |
| CN114805928A (en) * | 2022-03-10 | 2022-07-29 | 江苏森禾化工科技有限公司 | Metabenzene bio-based plasticizer |
| CN114805928B (en) * | 2022-03-10 | 2023-10-03 | 江苏森禾化工科技有限公司 | Biological base plasticizer for metaphenylene |
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