CN107057149A - Car light-weight environment-friendly type canister connecting tube and preparation method thereof - Google Patents
Car light-weight environment-friendly type canister connecting tube and preparation method thereof Download PDFInfo
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- CN107057149A CN107057149A CN201611272532.6A CN201611272532A CN107057149A CN 107057149 A CN107057149 A CN 107057149A CN 201611272532 A CN201611272532 A CN 201611272532A CN 107057149 A CN107057149 A CN 107057149A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
Abstract
The invention discloses a kind of car light-weight environment-friendly type canister connecting tube and preparation method thereof, using polyethylene, polyacrylamide as primary raw material, by adding rational material, melting is compound to obtain car light-weight environment-friendly type canister connecting tube raw material, solves the problem of existing car light-weight environment-friendly type canister connection tube material is heat-resisting poor.The invention surface of inorganic particles coat organic matter, compound particle surface organic matter prepared according to the methods of the invention is evenly distributed, and with reactivity, not only promote the dispersiveness of inorganic particulate in the plastic, and beneficial to the cross-linked network that stabilization is formed between organic matter, more it is mainly, will not forming properties defect point after micromolecular compound reaction.Car light-weight environment-friendly type canister connecting tube prepared by the present invention has outstanding machinability, has less density with more good heat resistance, and than existing car light-weight environment-friendly type canister connecting tube, beneficial to industrial applications.
Description
Technical field
The invention belongs to technical field of automobile accessories, and in particular to a kind of car with light-weight environment-friendly type canister connecting tube and its
Preparation method.
Background technology
Due to the shortcoming of easy aging of light plastic product itself, often occurs plastic crushing during use.Existing skill
The finished product of art has higher impact strength, but tensile strength is not high, and heat resistance is poor, it is impossible to meet automobile canister connection
The application of pipe.
The content of the invention
It is an object of the invention to provide a kind of car light-weight environment-friendly type canister connecting tube and preparation method thereof, with excellent
Heat resistance and good processability.
To achieve the above object of the invention, the technical solution adopted by the present invention is：
A kind of car preparation method of light-weight environment-friendly type canister connecting tube, comprises the following steps：
(1) 4- cyano group -4- (thio benzoylthio) valeric acid, methanol and polyethylene glycol is mixed；Then 4- diformazan ammonia is added
Yl pyridines, stirring adds maleic anhydride and azo dicyclohexyl formonitrile HCN hydrochloride, first time microwave reaction after 2 hours；Then
TPAOH is added, is reacted at room temperature 26 hours；Then di-sec-butyl peroxycarbonates are added and obtain mixed liquor；Again plus
Enter glycerine poly glycidyl ester, diethyl phosphite, tert-butyl hydroperoxide laurate；120~135 DEG C of stirrings 30~35 are small
Shi Hou, revolving removes solvent, is dried to obtain epoxide；
(2) polystyrene microsphere is dispersed in deionized water, stirring adds propilolic alcohol after 10~15 minutes；Then stir
30~40 minutes, add sodium bicarbonate and adjust pH value to 8.5；Then tetraethoxysilane is added, is stirred 20~30 minutes, Ran Houjia
Enter 3- aminopropyl triethoxysilanes and butyl borate, stir 10~20 minutes, be subsequently added into zinc citrate；50~55 DEG C
Stirring 70~80 minutes；Then filter, filter cake is washed with deionized and obtains solids again after being washed with acetone；Solids passes through
Powder is obtained after heat treatment；Powder is dissolved in n-hexane, amino-terminated Aqueous Solutions of Polyethylene Glycol and calcium sulfate water is added
Solution, after 80~95 DEG C are stirred 30~35 hours, filtration drying obtains compounded mix；
(3) polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate are well mixed, added through screw rod melting
Work, prepares olefin particles；Then olefin particles, polyvinyl, dimethyl tin oxide, epoxide are mixed equal
It is even, compositions of olefines is obtained, then by the standby just pipe of extrusion mechanism, eventually pass steam treatment and obtain car light-weight environment-friendly type carbon
Tank connecting tube.
In above-mentioned technical proposal, in step (1), 4- cyano group -4- (thio benzoylthio) valeric acid, methanol, polyethylene glycol,
DMAP, maleic anhydride, azo dicyclohexyl formonitrile HCN hydrochloride, TPAOH, di-sec-butyl peroxide
It is 100 to change carbonic ester, glycerine poly glycidyl ester, diethyl phosphite, the mass ratio of tert-butyl hydroperoxide laurate:
500: (12~18): (8~12): (15~23): (1~1.2): (3~5): (32~45): (160~180): (45~56):
(0.1~0.15).Epoxy resin has excellent performance, but processability is mismatched with alkene, and existing method of modifying is not
Beneficial to the compound of epoxy and alkene, it can not especially improve its processability, the epoxy prepolymer that the present invention is obtained not only is activated
Epoxy radicals, and carbonic ester segment and epoxy segment are combined, while connecting P element, obtained epoxy prepolymer has with alkene
There is approximate processability, it is ensured that the uniformity of W-response, while beneficial to the compound of thermosetting plastics' resin.
In plastics research and production process, usually using inorganic additive, this can not only reduce the cost of product, and
Some performances of plastic products can also be improved；However, because inorganic filler and organic polymer are in chemical constitution and physical aspect
On there is significant difference, both lack compatibility, often make the mechanical property and moulding processability of plastic products by
To influence.The present invention makes surface of inorganic particles become lipophile by hydrophily by adding the modification compounded mix especially compounded,
So as to improve the combination property of composite plastics material.
In above-mentioned technical proposal, in step (2), the Technology for Heating Processing is+500 DEG C/3 hours 200 DEG C/6 hours+850
DEG C/1 hour；The molecular weight of the amino-terminated polyethylene glycol is 3000~10000；Powder, amino-terminated polyethylene glycol,
The mass ratio of calcium sulfate is 100: (80~95): (10~19)；Polystyrene microsphere, propilolic alcohol, tetraethoxysilane, 3- ammonia third
Ethyl triethoxy silicane alkane, butyl borate, the mass ratio of zinc citrate are 100: (60~78): (58~65): 120: (41~
55)∶0.8.The present invention prepares inorganic powder by the technique of polymerization, sintering, and particle diameter distribution is narrow, while having porous knot
Structure, especially, hole wall have organic matter, are conducive to the interfacial reaction of melt stage organic matter and inorganic matter, increase organic-inorganic
The stability of system, while the presence of loose structure, contributes to density of material to decline, it is important to, mechanical property, heat resistance according to
It is so good.
In above-mentioned technical proposal, in step (3), polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate
Mass ratio be 10: 8: (6~8): (2~4)；Olefin particles, polyvinyl, dimethyl tin oxide, epoxide
Mass ratio is 100: (22~25): (2~3): (50~55).The method comprises the steps of firstly, preparing modified olefin, it is ensured that main material alkene
Performance uniformity, while the compounded mix for coating organic matter layer is pre-mixed with alkene, then with being answered with Modified Polymer
Close, under micromolecular compound improvement, modifying agent is crosslinked for alkene formation, greatly improves its resistant of high or low temperature, mechanical property,
Obtain good machinability and anti-flammability simultaneously.
In above-mentioned technical proposal, in step (3), the reactive extrursion temperature of screw rod melt-processed is 170~180 DEG C, screw rod
Rotating speed control is 110~115 revs/min, and residence time of the material in screw rod is 2~3 minutes；Melting temperature is 220 during extrusion
~230 DEG C, the time is 130~150 seconds；The temperature of steam treatment is 170~180 DEG C, and the time is 10~20 seconds, pressure 5~
5.5Bar。
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
(1) present invention is used using polyethylene, polyacrylamide as primary raw material, and by adding rational material, melting is multiple
Conjunction obtains car light-weight environment-friendly type canister connecting tube raw material, solves existing car light-weight environment-friendly type canister connection tubing
The problem of expecting resistance to heat differential.
(2) the invention surface of inorganic particles coat organic matter, compound grain prepared according to the methods of the invention
Sublist face organic compounds distribution is uniform, and with reactivity, not only promotes the dispersiveness of inorganic particulate in the plastic, and
Beneficial to stable cross-linked network is formed between organic matter, more it is mainly, will not forming properties defect after micromolecular compound reaction
Point.
(3) car light-weight environment-friendly type canister connecting tube prepared by the present invention has outstanding machinability, with more well
Heat resistance, and there is less density than existing car light-weight environment-friendly type canister connecting tube, should beneficial to industrialization
With.
Embodiment
With reference to embodiment, the invention will be further described：
A kind of car of embodiment one preparation method of light-weight environment-friendly type canister connecting tube, comprises the following steps：
(1) 4- cyano group -4- (thio benzoylthio) valeric acid, methanol and polyethylene glycol is mixed；Then 4- diformazan ammonia is added
Yl pyridines, stirring adds maleic anhydride and azo dicyclohexyl formonitrile HCN hydrochloride, first time microwave reaction after 2 hours；Then
TPAOH is added, is reacted at room temperature 26 hours；Then di-sec-butyl peroxycarbonates are added and obtain mixed liquor；Again plus
Enter glycerine poly glycidyl ester, diethyl phosphite, tert-butyl hydroperoxide laurate；After 135 DEG C are stirred 35 hours, revolving
Solvent is removed, epoxide is dried to obtain；4- cyano group -4- (thio benzoylthio) valeric acid, methanol, polyethylene glycol, 4- bis-
Methylamino pyridine, maleic anhydride, azo dicyclohexyl formonitrile HCN hydrochloride, TPAOH, di-sec-butyl peroxidating carbon
Acid esters, glycerine poly glycidyl ester, diethyl phosphite, the mass ratio of tert-butyl hydroperoxide laurate are 100: 500: 12
∶8∶15∶1∶3∶32∶160∶45∶0.1；
(2) polystyrene microsphere is dispersed in deionized water, stirring adds propilolic alcohol after 10 minutes；Then 30 points are stirred
Clock, adds sodium bicarbonate and adjusts pH value to 8.5；Then tetraethoxysilane is added, stirs 20 minutes, then adds 3- aminopropyls three
Ethoxysilane and butyl borate, stir 10 minutes, are subsequently added into zinc citrate；50 DEG C are stirred 70 minutes；Then filter,
Filter cake is washed with deionized and obtains solids again after being washed with acetone；Solids by+500 DEG C/3 hours 200 DEG C/6 hours+
Powder is obtained after heat treatment in 850 DEG C/1 hour；Powder is dissolved in n-hexane, amino-terminated polyethylene glycol (molecular weight is added
For the 3000) aqueous solution and the calcium sulfate aqueous solution, after 80 DEG C are stirred 30 hours, filtration drying obtains compounded mix；Powder, amino
The polyethylene glycol of end-blocking, the mass ratio of calcium sulfate are 100: 80: 10；Polystyrene microsphere, propilolic alcohol, tetraethoxysilane, 3-
Aminopropyl triethoxysilane, butyl borate, the mass ratio of zinc citrate are 100: 60: 58: 120: 41: 0.8；
(3) polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate are well mixed, added through screw rod melting
Work, prepares olefin particles；Then olefin particles, polyvinyl, dimethyl tin oxide, epoxide are mixed equal
It is even, compositions of olefines is obtained, then by the standby just pipe of extrusion mechanism, eventually pass steam treatment and obtain car light-weight environment-friendly type carbon
Tank connecting tube；Polyethylene, polyacrylamide, compounded mix, the mass ratio of polymethyl methacrylate are 10: 8: 6: 2；Alkene grain
Son, polyvinyl, dimethyl tin oxide, the mass ratio of epoxide are 100: 22: 2: 50.
The reactive extrursion temperature of screw rod melt-processed is 170~180 DEG C, and screw speed control is 115 revs/min, and material exists
Residence time in screw rod is 2 minutes；Melting temperature is 220~230 DEG C during extrusion, and the time is 130 seconds；The temperature of steam treatment
For 170 DEG C, the time is 10 seconds, pressure 5Bar.
Tested according to TL52655-B, the glass transition temperature of above-mentioned car high-low temperature resistant antiseep breather pipe is 151
DEG C, oxygen index (OI) is 29, hardness 65, tensile strength 29N/mm2, elongation at break 154%, fire resistant oil gas, five circulations, surface
Nothing opens bubble, density 1.01g/cm3。
A kind of car of embodiment two preparation method of light-weight environment-friendly type canister connecting tube, comprises the following steps：
(1) 4- cyano group -4- (thio benzoylthio) valeric acid, methanol and polyethylene glycol is mixed；Then 4- diformazan ammonia is added
Yl pyridines, stirring adds maleic anhydride and azo dicyclohexyl formonitrile HCN hydrochloride, first time microwave reaction after 2 hours；Then
TPAOH is added, is reacted at room temperature 26 hours；Then di-sec-butyl peroxycarbonates are added and obtain mixed liquor；Again plus
Enter glycerine poly glycidyl ester, diethyl phosphite, tert-butyl hydroperoxide laurate；120~135 DEG C of stirrings 30~35 are small
Shi Hou, revolving removes solvent, is dried to obtain epoxide；4- cyano group -4- (thio benzoylthio) valeric acid, methanol, poly- second
Glycol, DMAP, maleic anhydride, azo dicyclohexyl formonitrile HCN hydrochloride, TPAOH, di-sec-butyl
Peroxycarbonates, glycerine poly glycidyl ester, diethyl phosphite, the mass ratio of tert-butyl hydroperoxide laurate are
100∶500∶18∶12∶23∶1.2∶5∶45∶180∶56∶0.15；
(2) polystyrene microsphere is dispersed in deionized water, stirring adds propilolic alcohol after 15 minutes；Then 30 points are stirred
Clock, adds sodium bicarbonate and adjusts pH value to 8.5；Then tetraethoxysilane is added, stirs 20 minutes, then adds 3- aminopropyls three
Ethoxysilane and butyl borate, stir 10 minutes, are subsequently added into zinc citrate；55 DEG C are stirred 80 minutes；Then filter,
Filter cake is washed with deionized and obtains solids again after being washed with acetone；Solids by+500 DEG C/3 hours 200 DEG C/6 hours+
Powder is obtained after heat treatment in 850 DEG C/1 hour；Powder is dissolved in n-hexane, amino-terminated polyethylene glycol (molecular weight is added
For the 10000) aqueous solution and the calcium sulfate aqueous solution, after 85 DEG C are stirred 30 hours, filtration drying obtains compounded mix；Powder, ammonia
The polyethylene glycol of base end-blocking, the mass ratio of calcium sulfate are 100: 95: 19；Polystyrene microsphere, propilolic alcohol, tetraethoxysilane,
3- aminopropyl triethoxysilanes, butyl borate, the mass ratio of zinc citrate are 100: 78: 65: 120: 55: 0.8；
(3) polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate are well mixed, added through screw rod melting
Work, prepares olefin particles；Then olefin particles, polyvinyl, dimethyl tin oxide, epoxide are mixed equal
It is even, compositions of olefines is obtained, then by the standby just pipe of extrusion mechanism, eventually pass steam treatment and obtain car light-weight environment-friendly type carbon
Tank connecting tube；Polyethylene, polyacrylamide, compounded mix, the mass ratio of polymethyl methacrylate are 10: 8: 8: 4；Alkene grain
Son, polyvinyl, dimethyl tin oxide, the mass ratio of epoxide are 100: 25: 3: 55.
The reactive extrursion temperature of screw rod melt-processed is 170~180 DEG C, and screw speed control is 110 revs/min, and material exists
Residence time in screw rod is 3 minutes；Melting temperature is 220~230 DEG C during extrusion, and the time is 130 seconds；The temperature of steam treatment
For 180 DEG C, the time is 10 seconds, pressure 5.5Bar.
Tested according to TL52655-B, the glass transition temperature of above-mentioned car high-low temperature resistant antiseep breather pipe is 153
DEG C, oxygen index (OI) is 29, hardness 66, tensile strength 30N/mm2, elongation at break 148%, fire resistant oil gas, five circulations, surface
Nothing opens bubble, density 1.01g/cm3。
A kind of car of embodiment three preparation method of light-weight environment-friendly type canister connecting tube, comprises the following steps：
(1) 4- cyano group -4- (thio benzoylthio) valeric acid, methanol and polyethylene glycol is mixed；Then 4- diformazan ammonia is added
Yl pyridines, stirring adds maleic anhydride and azo dicyclohexyl formonitrile HCN hydrochloride, first time microwave reaction after 2 hours；Then
TPAOH is added, is reacted at room temperature 26 hours；Then di-sec-butyl peroxycarbonates are added and obtain mixed liquor；Again plus
Enter glycerine poly glycidyl ester, diethyl phosphite, tert-butyl hydroperoxide laurate；After 125 DEG C are stirred 30 hours, revolving
Solvent is removed, epoxide is dried to obtain；4- cyano group -4- (thio benzoylthio) valeric acid, methanol, polyethylene glycol, 4- bis-
Methylamino pyridine, maleic anhydride, azo dicyclohexyl formonitrile HCN hydrochloride, TPAOH, di-sec-butyl peroxidating carbon
Acid esters, glycerine poly glycidyl ester, diethyl phosphite, the mass ratio of tert-butyl hydroperoxide laurate are 100: 500: 12
∶8∶15∶1∶3∶32∶160∶45∶0.1；
(2) polystyrene microsphere is dispersed in deionized water, stirring adds propilolic alcohol after 10 minutes；Then 35 points are stirred
Clock, adds sodium bicarbonate and adjusts pH value to 8.5；Then tetraethoxysilane is added, stirs 25 minutes, then adds 3- aminopropyls three
Ethoxysilane and butyl borate, stir 15 minutes, are subsequently added into zinc citrate；50 DEG C are stirred 75 minutes；Then filter,
Filter cake is washed with deionized and obtains solids again after being washed with acetone；Solids by+500 DEG C/3 hours 200 DEG C/6 hours+
Powder is obtained after heat treatment in 850 DEG C/1 hour；Powder is dissolved in n-hexane, amino-terminated polyethylene glycol (molecular weight is added
For the 8000) aqueous solution and the calcium sulfate aqueous solution, after 95 DEG C are stirred 30 hours, filtration drying obtains compounded mix；Powder, amino
The polyethylene glycol of end-blocking, the mass ratio of calcium sulfate are 100: 95: 19；Polystyrene microsphere, propilolic alcohol, tetraethoxysilane, 3-
Aminopropyl triethoxysilane, butyl borate, the mass ratio of zinc citrate are 100: 78: 65: 120: 55: 0.8；
(3) polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate are well mixed, added through screw rod melting
Work, prepares olefin particles；Then olefin particles, polyvinyl, dimethyl tin oxide, epoxide are mixed equal
It is even, compositions of olefines is obtained, then by the standby just pipe of extrusion mechanism, eventually pass steam treatment and obtain car light-weight environment-friendly type carbon
Tank connecting tube；Polyethylene, polyacrylamide, compounded mix, the mass ratio of polymethyl methacrylate are 10: 8: 8: 4；Alkene grain
Son, polyvinyl, dimethyl tin oxide, the mass ratio of epoxide are 100: 25: 3: 55.Screw rod melt-processed it is anti-
It is 170~180 DEG C to answer extrusion temperature, and screw speed control is 110 revs/min, and residence time of the material in screw rod is 3 minutes；
Melting temperature is 220~230 DEG C during extrusion, and the time is 130 seconds；The temperature of steam treatment is 170 DEG C, and the time is 10 seconds, pressure
5.5Bar。
Tested according to TL52655-B, the glass transition temperature of above-mentioned car high-low temperature resistant antiseep breather pipe is 149
DEG C, oxygen index (OI) is 29, hardness 66, tensile strength 28N/mm2, elongation at break 159%, fire resistant oil gas, five circulations, surface
Nothing opens bubble, density 1.02g/cm3。
A kind of car of example IV preparation method of light-weight environment-friendly type canister connecting tube, comprises the following steps：
(1) 4- cyano group -4- (thio benzoylthio) valeric acid, methanol and polyethylene glycol is mixed；Then 4- diformazan ammonia is added
Yl pyridines, stirring adds maleic anhydride and azo dicyclohexyl formonitrile HCN hydrochloride after 2 hours, first time microwave reaction is conventional
Power；Then TPAOH is added, is reacted at room temperature 26 hours；Then di-sec-butyl peroxycarbonates are added to be mixed
Close liquid；Add glycerine poly glycidyl ester, diethyl phosphite, tert-butyl hydroperoxide laurate；135 DEG C of stirrings 30 are small
Shi Hou, revolving removes solvent, is dried to obtain epoxide；4- cyano group -4- (thio benzoylthio) valeric acid, methanol, poly- second
Glycol, DMAP, maleic anhydride, azo dicyclohexyl formonitrile HCN hydrochloride, TPAOH, di-sec-butyl
Peroxycarbonates, glycerine poly glycidyl ester, diethyl phosphite, the mass ratio of tert-butyl hydroperoxide laurate are
100∶500∶18∶12∶23∶1.2∶5∶45∶180∶56∶0.15；
(2) polystyrene microsphere is dispersed in deionized water, stirring adds propilolic alcohol after 15 minutes；Then 30 points are stirred
Clock, adds sodium bicarbonate and adjusts pH value to 8.5；Then tetraethoxysilane is added, stirs 25 minutes, then adds 3- aminopropyls three
Ethoxysilane and butyl borate, stir 10 minutes, are subsequently added into zinc citrate；55 DEG C are stirred 70 minutes；Then filter,
Filter cake is washed with deionized and obtains solids again after being washed with acetone；Solids by+500 DEG C/3 hours 200 DEG C/6 hours+
Powder is obtained after heat treatment in 850 DEG C/1 hour；Powder is dissolved in n-hexane, amino-terminated polyethylene glycol (molecular weight is added
For the 5000) aqueous solution and the calcium sulfate aqueous solution, after 95 DEG C are stirred 30 hours, filtration drying obtains compounded mix；Powder, amino
The polyethylene glycol of end-blocking, the mass ratio of calcium sulfate are 100: 80: 10；Polystyrene microsphere, propilolic alcohol, tetraethoxysilane, 3-
Aminopropyl triethoxysilane, butyl borate, the mass ratio of zinc citrate are 100: 60: 58: 120: 41: 0.8；
(3) polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate are well mixed, added through screw rod melting
Work, prepares olefin particles；Then olefin particles, polyvinyl, dimethyl tin oxide, epoxide are mixed equal
It is even, compositions of olefines is obtained, then by the standby just pipe of extrusion mechanism, eventually pass steam treatment and obtain car light-weight environment-friendly type carbon
Tank connecting tube；Polyethylene, polyacrylamide, compounded mix, the mass ratio of polymethyl methacrylate are 10: 8: 6: 2；Alkene grain
Son, polyvinyl, dimethyl tin oxide, the mass ratio of epoxide are 100: 22: 2: 50.
The reactive extrursion temperature of screw rod melt-processed is 170~180 DEG C, and screw speed control is 115 revs/min, and material exists
Residence time in screw rod is 3 minutes；Melting temperature is 220~230 DEG C during extrusion, and the time is 140 seconds；The temperature of steam treatment
For 180 DEG C, the time is 15 seconds, pressure 5.5Bar.
Tested according to TL52655-B, the glass transition temperature of above-mentioned car high-low temperature resistant antiseep breather pipe is 152
DEG C, oxygen index (OI) is 29, hardness 65, tensile strength 31N/mm2, elongation at break 144%, fire resistant oil gas, five circulations, surface
Nothing opens bubble, density 1.01g/cm3。
Embodiment five
(1) 4- cyano group -4- (thio benzoylthio) valeric acid, methanol and polyethylene glycol is mixed；Then 4- diformazan ammonia is added
Yl pyridines, stirring adds maleic anhydride and azo dicyclohexyl formonitrile HCN hydrochloride, first time microwave reaction after 2 hours；Then
TPAOH is added, is reacted at room temperature 26 hours；Then di-sec-butyl peroxycarbonates are added and obtain mixed liquor；Again plus
Enter glycerine poly glycidyl ester, diethyl phosphite, tert-butyl hydroperoxide laurate；After 130 DEG C are stirred 35 hours, revolving
Solvent is removed, epoxide is dried to obtain；4- cyano group -4- (thio benzoylthio) valeric acid, methanol, polyethylene glycol, 4- bis-
Methylamino pyridine, maleic anhydride, azo dicyclohexyl formonitrile HCN hydrochloride, TPAOH, di-sec-butyl peroxidating carbon
Acid esters, glycerine poly glycidyl ester, diethyl phosphite, the mass ratio of tert-butyl hydroperoxide laurate are 100: 500: 12
∶8∶15∶1∶3∶32∶160∶45∶0.1；
(2) polystyrene microsphere is dispersed in deionized water, stirring adds propilolic alcohol after 15 minutes；Then 30 points are stirred
Clock, adds sodium bicarbonate and adjusts pH value to 8.5；Then tetraethoxysilane is added, stirs 20 minutes, then adds 3- aminopropyls three
Ethoxysilane and butyl borate, stir 10 minutes, are subsequently added into zinc citrate；50 DEG C are stirred 70 minutes；Then filter,
Filter cake is washed with deionized and obtains solids again after being washed with acetone；Solids by+500 DEG C/3 hours 200 DEG C/6 hours+
Powder is obtained after heat treatment in 850 DEG C/1 hour；Powder is dissolved in n-hexane, amino-terminated polyethylene glycol (molecular weight is added
For the 6000) aqueous solution and the calcium sulfate aqueous solution, after 95 DEG C are stirred 30 hours, filtration drying obtains compounded mix；Powder, amino
The polyethylene glycol of end-blocking, the mass ratio of calcium sulfate are 100: 80: 10；Polystyrene microsphere, propilolic alcohol, tetraethoxysilane, 3-
Aminopropyl triethoxysilane, butyl borate, the mass ratio of zinc citrate are 100: 60: 58: 120: 41: 0.8；
(3) polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate are well mixed, added through screw rod melting
Work, prepares olefin particles；Then olefin particles, polyvinyl, dimethyl tin oxide, epoxide are mixed equal
It is even, compositions of olefines is obtained, then by the standby just pipe of extrusion mechanism, eventually pass steam treatment and obtain car light-weight environment-friendly type carbon
Tank connecting tube；Polyethylene, polyacrylamide, compounded mix, the mass ratio of polymethyl methacrylate are 10: 8: 8: 4；Alkene grain
Son, polyvinyl, dimethyl tin oxide, the mass ratio of epoxide are 100: 25: 3: 55.
The reactive extrursion temperature of screw rod melt-processed is 170~180 DEG C, and screw speed control is 110 revs/min, and material exists
Residence time in screw rod is 3 minutes；Melting temperature is 220~230 DEG C during extrusion, and the time is 130 seconds；The temperature of steam treatment
For 180 DEG C, the time is 10 seconds, pressure 5Bar.
Tested according to TL52655-B, the glass transition temperature of above-mentioned car high-low temperature resistant antiseep breather pipe is 157
DEG C, oxygen index (OI) is 29, hardness 64, tensile strength 32N/mm2, elongation at break 147%, fire resistant oil gas, five circulations, surface
Nothing opens bubble, density 1.01g/cm3。
Claims (10)
1. a kind of car preparation method of light-weight environment-friendly type canister connecting tube, it is characterised in that comprise the following steps：
(1) 4- cyano group -4- (thio benzoylthio) valeric acid, methanol and polyethylene glycol is mixed；Then 4- dimethylamino pyrroles are added
Pyridine, stirring adds maleic anhydride and azo dicyclohexyl formonitrile HCN hydrochloride, first time microwave reaction after 2 hours；Then add
TPAOH, is reacted at room temperature 26 hours；Then di-sec-butyl peroxycarbonates are added and obtain mixed liquor；Add third
Triol poly glycidyl ester, diethyl phosphite, tert-butyl hydroperoxide laurate；120~135 DEG C are stirred 30~35 hours
Afterwards, revolving removes solvent, is dried to obtain epoxide；
(2) polystyrene microsphere is dispersed in deionized water, stirring adds propilolic alcohol after 10~15 minutes；Then stirring 30~
40 minutes, add sodium bicarbonate and adjust pH value to 8.5；Then tetraethoxysilane is added, stirs 20~30 minutes, then adds 3-
Aminopropyl triethoxysilane and butyl borate, stir 10~20 minutes, are subsequently added into zinc citrate；50~55 DEG C of stirrings
70~80 minutes；Then filter, filter cake is washed with deionized and obtains solids again after being washed with acetone；Solids through overheat at
Powder is obtained after reason；Powder is dissolved in n-hexane, amino-terminated Aqueous Solutions of Polyethylene Glycol and the calcium sulfate aqueous solution is added,
After 80~95 DEG C are stirred 30~35 hours, filtration drying obtains compounded mix；
(3) polyethylene, polyacrylamide, compounded mix, polymethyl methacrylate are well mixed, through screw rod melt-processed,
Prepare olefin particles；Then olefin particles, polyvinyl, dimethyl tin oxide, epoxide are well mixed,
Compositions of olefines is obtained, then by the standby just pipe of extrusion mechanism, eventually passes steam treatment and obtains car light-weight environment-friendly type canister
Connecting tube.
2. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(1) in, 4- cyano group -4- (thio benzoylthio) valeric acid, methanol, polyethylene glycol, DMAP, maleic anhydride, idol
Nitrogen diisopropyl imidazoline hydrochloride, TPAOH, di-sec-butyl peroxycarbonates, glycerine poly epihydric alcohol
Ester, diethyl phosphite, the mass ratio of tert-butyl hydroperoxide laurate are 100: 500: (12~18): (8~12): (15~
23): (1~1.2): (3~5): (32~45): (160~180): (45~56): (0.1~0.15).
3. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(2) in, the Technology for Heating Processing is+850 DEG C/1 hour+500 DEG C/3 hours 200 DEG C/6 hours；The amino-terminated poly- second
The molecular weight of glycol is 3000~10000.
4. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(2) in, powder, amino-terminated polyethylene glycol, the mass ratio of calcium sulfate are 100: (80~95): (10~19).
5. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(2) in, polystyrene microsphere, propilolic alcohol, tetraethoxysilane, 3- aminopropyl triethoxysilanes, butyl borate, citric acid
The mass ratio of zinc is 100: (60~78): (58~65): 120: (41~55): 0.8.
6. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(3) in, polyethylene, polyacrylamide, compounded mix, the mass ratio of polymethyl methacrylate are 10: 8: (6~8): (2~
4)；Olefin particles, polyvinyl, dimethyl tin oxide, the mass ratio of epoxide are 100: (22~25): (2~3)
: (50~55).
7. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(3) in, the reactive extrursion temperature of screw rod melt-processed is 170~180 DEG C, and screw speed control is 110~115 revs/min, material
Residence time in screw rod is 2~3 minutes.
8. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(3) in, melting temperature is 220~230 DEG C during extrusion, and the time is 130~150 seconds.
9. the preparation method of car light-weight environment-friendly type canister connecting tube according to claim 1, it is characterised in that：Step
(3) in, the temperature of steam treatment is 170~180 DEG C, and the time is 10~20 seconds, 5~5.5Bar of pressure.
10. the car light-weight environment-friendly that car described in claim 1 is prepared with the preparation method of light-weight environment-friendly type canister connecting tube
Type canister connecting tube.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611272532.6A CN107057149A (en) | 2016-12-29 | 2016-12-29 | Car light-weight environment-friendly type canister connecting tube and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611272532.6A CN107057149A (en) | 2016-12-29 | 2016-12-29 | Car light-weight environment-friendly type canister connecting tube and preparation method thereof |
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ID=59624377
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367973A (en) * | 2008-10-09 | 2009-02-18 | 上海交通大学 | Preparation method for high-strength heat-proof polythene composite material |
| CN105924751A (en) * | 2016-07-04 | 2016-09-07 | 常州瑞杰新材料科技股份有限公司 | HDPE composite material resistant to environmental stress cracking for hollow container |
| CN106084426A (en) * | 2016-08-08 | 2016-11-09 | 涂瑞强 | A kind of silicon oil modified PE pipeline and preparation method thereof |
-
2016
- 2016-12-29 CN CN201611272532.6A patent/CN107057149A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367973A (en) * | 2008-10-09 | 2009-02-18 | 上海交通大学 | Preparation method for high-strength heat-proof polythene composite material |
| CN105924751A (en) * | 2016-07-04 | 2016-09-07 | 常州瑞杰新材料科技股份有限公司 | HDPE composite material resistant to environmental stress cracking for hollow container |
| CN106084426A (en) * | 2016-08-08 | 2016-11-09 | 涂瑞强 | A kind of silicon oil modified PE pipeline and preparation method thereof |
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Address after: Jiangyin City, Jiangsu Province town of Hua 214421 Huaxi Village nine Mongolia Nalu No. 1 Applicant after: Jiangyin automotive components Limited by Share Ltd Address before: Jiangyin City, Jiangsu Province town of Hua 214421 Huaxi Village nine Mongolia Nalu No. 1 Applicant before: Jiangyin Biaobang Auto Parts Co., Ltd. |
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