CN109233063A - A kind of heat-resisting masterbatch of hot water plastic tube special graphite alkene and preparation method - Google Patents
A kind of heat-resisting masterbatch of hot water plastic tube special graphite alkene and preparation method Download PDFInfo
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- C08J3/20—Compounding polymers with additives, e.g. colouring
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Abstract
The invention discloses a kind of heat-resisting masterbatch of hot water plastic tube special graphite alkene and preparation methods.Preparation step are as follows: ethyl orthosilicate a, is dissolved in deionized water and is adjusted pH value, teos solution is made；B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution, heating washs drying after being stirred to react, and pulverizes, and the coated porous calcium phosphate composite powder of Silica hydrogel is made；C, with polymer, dispersant extruding pelletization, the heat-resisting masterbatch of graphene will be made after composite powder infiltration organic solvent.The method has the advantages that preparation method effective solution of the invention graphene problem easy to reunite, it can guarantee that graphene is evenly dispersed in plastic substrate, improve the uniformity of plastic products, gained plastic products have excellent heat resistance and mechanical property, and preparation process is simple, it is at low cost, it can be applicable.
Description
Technical field
The present invention relates to plastic matrix fields, and in particular to the preparation of heat-resisting masterbatch, more particularly, to a kind of hot water plastics
The heat-resisting masterbatch of pipe special graphite alkene and preparation method.
Background technique
Stabilizer, lubricant, plasticizer is added usually with synthetic resin, that is, using polymer as raw material in plastic tube
Deng being formed by the extrusion process of plastic compression machine.Due to plastic tube have light, corrosion-resistant, good appearance, without bad smell, plus
The features such as work is easy, is easy for construction, is more and more widely used in construction projects.It is mainly used as building construction
Tap water supply system piping, draining, exhaust and blowdown sanitary pipe, subsoil drain system, rain pipe and electric wire installation are matched
The penetration pipe etc. applied.
Polyvinyl resin has excellent low temperature resistance and processability as one of thermoplastic resin the most general
Energy.But the limitation that polyethylene also has it to use, such as the intensity of common polythene is not high, under normal circumstances, compares polypropylene
Intensity want low.And polyethylene products cannot all be used for a long time in the environment of being higher than 50 DEG C under normal circumstances.For linear
For polyethylene, molecular weight is bigger, and strand is longer, and crystalline rate can be relatively slack-off, this interaction between molecule
There is very big relationship with tangling.Graphene as the novel high performance material of one kind applied in recent years, have enhancing, it is thermally conductive,
A variety of unique physical and chemical performances such as heat-resisting, big specific surface area, strong interface interaction, show huge application potential.
Number of patent application 201711043783.1 discloses a kind of multi-functional tubing based on graphene and polyethylene, including
Following raw material: polyvinyl resin, graphene, phenolic resin, fire retardant, aluminium hydroxide, silicon systems material, magnesium salt whisker, glass fibers
Dimension, methyl vinyl silicone rubber, gas-phase silica, calcinated argil, schmigel, epoxy resin, pentaerythritol stearate, benzene oxygen
It is base polyphosphazene elastomer, flame-retardant master batch, nano-silicon nitride, antioxidant, expanding material, propylene, 1- butylene, 1- hexene, stearic acid, micro-
Spar wax and zinc oxide.The invention preparation the multi-functional tubing based on graphene and polyethylene have high temperature resistant, radiation protection,
There is excellent mechanical property under the conditions of high temperature and humidity, be suitble to use in the extreme condition environment full of radiation.
Number of patent application 201710408671.5 discloses a kind of graphene enhancing heat-proof polythene composite pipe and its system
Preparation Method, the main purpose of the invention are to solve general polyvinyl piping materials non-refractory, are easy damaged technical problem, provide
A kind of graphene enhances heat-proof polythene composite pipe, the component including following parts by weight: the resistance to hot polymerization of hervene copolymer high density
80 ~ 90 parts of ethylene, contains 2 ~ 4 parts of fluorobenzene ethene, 2 ~ 4 parts of coupling agent, 6 ~ 8 parts of plasticizer, antioxidant 1 ~ 3 at 0.1 ~ 3 part of graphene
Part, 2 ~ 4 parts of lubricant, 10 ~ 30 parts of lytic agent, 0.1 ~ 0.3 part of surfactant, preparation method include dissolution, stirring, ultrasound,
Mixing, heating, single screw rod squeeze out and etc..
Number of patent application 201410190194.6 discloses a kind of heat-proof polythene composite pipe modified with graphene
Preparation method, step include: the preparation of (1) modified graphene powder；(2) modified graphene powder/heat-proof polythene is blended
The preparation of master batch；(3) with the preparation of the modified heat-proof polythene composite pipe of graphene.The invention makes full use of heat-proof polythene
Existing equipment in composite pipe industry only need to utilize graphene powder modified on a small quantity can be to tubing in conduction on formula
It is obviously improved in terms of performance, mechanical strength and anti-aging property, at low cost, effect is obvious, has very strong practicability.
Number of patent application 201310739948.4 discloses a kind of polyvinyl piping materials of high-intensitive heat-resistant, wear-resistant, the high intensity
The polyvinyl piping materials of heat-resistant, wear-resistant successively include: micron order modified ultra-high molecular weight polyethylene layer, high-density polyethylene from the inside to the outside
The macromolecule modified material layer of alkene and inorganic mineral, polyethylene carpet veneer, by weight, the raw material of polyethylene carpet veneer form are as follows:
100 parts of polyethylene；10 ~ 20 parts of nano material；1 ~ 3 part of compatilizer；1 ~ 3 part of toughener；1 ~ 2 part of coupling agent；Lubricant 1 ~
1.5 part；1 ~ 1.5 part of antioxidant.The advantages of the invention, is: it is fully dispersed in plastic resin by nanoparticle, effectively
Improve the performances such as heat-resisting, weather-proof, wear-resisting of plastics.
It can be seen that when addition graphene carries out enhancing modified in plastic tube preparation in the prior art, usually because of graphite
Alkene nanoparticle effect and easily reunite, be either directly used in plastics or prefabricated masterbatch, be required to decentralized processing, and show
The conventional dispersion means based on dispersing aid are difficult to effectively disperse graphene, so that its modifying function is limited,
Reinforcing effect is undesirable.
Summary of the invention
Effectively to solve above-mentioned technical problem, the invention proposes a kind of heat-resisting masterbatch of hot water plastic tube special graphite alkene and
Preparation method can effectively solve the problems, such as that graphene is easy to reunite, and plastic tube heat resistance and mechanical property obtained are good.
The specific technical solution of the present invention is as follows:
A kind of preparation method of the heat-resisting masterbatch of hot water plastic tube special graphite alkene, the heat-resisting masterbatch of graphene is by loading
The silicone-hydrogel of the porous calcium phosphate microsphere surface reaction cladding high-fire resistance of graphene, is further changed using organic solvent
Property, it is then made with mixed with polymers extruding pelletization at masterbatch, specific preparation step are as follows:
A, ethyl orthosilicate is dissolved in deionized water, adjusting pH value using ammonium hydroxide is 10, and teos solution is made；
B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution made from step a, heats up and stirs
Reaction, then adjusting pH value using acid solution is 6 ~ 7, is cooled down after reaction, filters, washs repeatedly, until the pH value of filtrate
It is 7, by much filtrate drying and pulverizes, the coated porous calcium phosphate composite powder of Silica hydrogel is made；
C, filtering, dry by the infiltration 2 ~ 3h in organic solvent of composite powder made from step b, further with polymer, dispersion
The heat-resisting masterbatch of graphene is made using double screw extruder extruding pelletization in agent mixing.
Preferably, in step a, 20 ~ 30 parts by weight of ethyl orthosilicate, 70 ~ 80 parts by weight of deionized water.
Preferably, in the step b, 8 ~ 12 parts by weight of graphene, 22 ~ 30 parts by weight of porous calcium phosphate microsphere, positive silicic acid
58 ~ 70 parts by weight of ethyl ester solution.
Preferably, in the step b, reaction temperature is 120 ~ 150 DEG C, and the time is 90 ~ 150min.
Preferably, in the step c, organic solvent is acetone, espeleton, methylisobutylketone, cyclohexanone, toluene hexamethylene
One of ketone, methyl acetate, ethyl acetate, propyl acetate, acetonitrile, pyridine.
Preferably, in the step c, polymer is one of polyethylene, polypropylene.
Preferably, in the step c, dispersing agent is zinc stearate, calcium stearate, magnesium stearate, copper stearate, stearic acid
At least one of sodium, potassium stearate.
Preferably, in step c, 30 ~ 40 parts by weight of composite powder, 57 ~ 69 parts by weight of polymer, 1 ~ 3 parts by weight of dispersing agent.
The present invention coats the silicone-hydrogel of high-fire resistance by the porous calcium phosphate microsphere surface reaction in load graphene,
Further modified and polymer prills are at masterbatch using organic solvent, graphene is closed in more by the silicone-hydrogel of microsphere surface
In the microballoon of hole, use is directly added when producing polyvinyl plastic pipeline, silicone-hydrogel is modified with plastics base by organic solvent
Body has excellent compatibility, be conducive to polyethylene macromolecular chain and mutually tangle with microballoon, and graphene is easy to reunite asks for effective solution
Topic.
Above content of the present invention also proposes a kind of heat-resisting masterbatch of hot water plastic tube special graphite alkene, is made by following steps:
A, ethyl orthosilicate is dissolved in deionized water and is adjusted pH value, teos solution is made；B, the more of graphene will be loaded
Hole calcium phosphate microsphere immerses in teos solution, and heating washs drying after being stirred to react, and pulverizes, and Silica hydrogel packet is made
Cover porous calcium phosphate composite powder；C, will be with polymer, dispersant extruding pelletization after composite powder infiltration organic solvent
It can be made.
The invention has the benefit that
1. proposing to load graphene using porous calcium phosphate microsphere and coat modification is carried out after silicone-hydrogel prepare hot water plastics
The method of the heat-resisting masterbatch of pipe special graphite alkene.
2. preparation method effective solution of the invention graphene problem easy to reunite, can guarantee the graphene in plastics
It is evenly dispersed in matrix, the uniformity of plastic products is improved, gained plastic products have excellent heat resistance and mechanics
Performance.
3. preparation process of the present invention is simple, at low cost, can be applicable.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A, ethyl orthosilicate is dissolved in deionized water, adjusting pH value using ammonium hydroxide is 10, and teos solution is made；Its
In, 25 parts by weight of ethyl orthosilicate, 75 parts by weight of deionized water；
B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution made from step a, heats up and stirs
Reaction, reaction temperature are 135 DEG C, time 120min, and then adjusting pH value using acid solution is 6.5, are cooled down after reaction,
It filters, wash repeatedly, until the pH value of filtrate is 7, by much filtrate drying and pulverizes, the coated porous phosphoric acid of Silica hydrogel is made
Calcium composite powder；Wherein, 10 parts by weight of graphene, 26 parts by weight of porous calcium phosphate microsphere, 64 parts by weight of teos solution；
C, filtering, dry by the infiltration 2.5h in organic solvent of composite powder made from step b, further with polymer, dispersion
Using double screw extruder extruding pelletization the heat-resisting masterbatch of graphene is made wherein, organic solvent is acetone, polymer in agent mixing
For polyethylene, dispersing agent is zinc stearate；35 parts by weight of composite powder, 63 parts by weight of polymer, 2 parts by weight of dispersing agent.
Embodiment 2
A, ethyl orthosilicate is dissolved in deionized water, adjusting pH value using ammonium hydroxide is 10, and teos solution is made；Its
In, 28 parts by weight of ethyl orthosilicate, 72 parts by weight of deionized water；
B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution made from step a, heats up and stirs
Reaction, reaction temperature are 140 DEG C, time 100min, and then adjusting pH value using acid solution is 7, are cooled down after reaction, instead
It filters again, washing, until the pH value of filtrate is 7, by much filtrate drying and pulverizes, the coated porous calcium phosphate of Silica hydrogel is made
Composite powder；Wherein, 11 parts by weight of graphene, 28 parts by weight of porous calcium phosphate microsphere, 61 parts by weight of teos solution；
C, filtering, dry by the infiltration 3h in organic solvent of composite powder made from step b, further with polymer, dispersing agent
The heat-resisting masterbatch of graphene is made using double screw extruder extruding pelletization in mixing；Wherein, organic solvent is espeleton, polymerization
Object is polypropylene, and dispersing agent is calcium stearate；37 parts by weight of composite powder, 60 parts by weight of polymer, 3 parts by weight of dispersing agent.
Embodiment 3
A, ethyl orthosilicate is dissolved in deionized water, adjusting pH value using ammonium hydroxide is 10, and teos solution is made；Its
In, 30 parts by weight of ethyl orthosilicate, 70 parts by weight of deionized water；
B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution made from step a, heats up and stirs
Reaction, reaction temperature are 150 DEG C, time 90min, and then adjusting pH value using acid solution is 6, are cooled down after reaction, instead
It filters again, washing, until the pH value of filtrate is 7, by much filtrate drying and pulverizes, the coated porous calcium phosphate of Silica hydrogel is made
Composite powder；Wherein, 12 parts by weight of graphene, 30 parts by weight of porous calcium phosphate microsphere, 58 parts by weight of teos solution；
C, filtering, dry by the infiltration 2h in organic solvent of composite powder made from step b, further with polymer, dispersing agent
The heat-resisting masterbatch of graphene is made using double screw extruder extruding pelletization in mixing；Wherein, organic solvent is methylisobutylketone, is gathered
Conjunction object is polyethylene, and dispersing agent is magnesium stearate；40 parts by weight of composite powder, 57 parts by weight of polymer, 3 parts by weight of dispersing agent.
Embodiment 4
A, ethyl orthosilicate is dissolved in deionized water, adjusting pH value using ammonium hydroxide is 10, and teos solution is made；Its
In, 23 parts by weight of ethyl orthosilicate, 77 parts by weight of deionized water；
B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution made from step a, heats up and stirs
Reaction, reaction temperature are 130 DEG C, time 130min, and then adjusting pH value using acid solution is 6, are cooled down after reaction, instead
It filters again, washing, until the pH value of filtrate is 7, by much filtrate drying and pulverizes, the coated porous calcium phosphate of Silica hydrogel is made
Composite powder；Wherein, 9 parts by weight of graphene, 25 parts by weight of porous calcium phosphate microsphere, 66 parts by weight of teos solution；
C, filtering, dry by the infiltration 2h in organic solvent of composite powder made from step b, further with polymer, dispersing agent
The heat-resisting masterbatch of graphene is made using double screw extruder extruding pelletization in mixing；Wherein, organic solvent is cyclohexanone, polymer
For polypropylene, dispersing agent is copper stearate；32 parts by weight of composite powder, 67 parts by weight of polymer, 1 parts by weight of dispersing agent.
Embodiment 5
A, ethyl orthosilicate is dissolved in deionized water, adjusting pH value using ammonium hydroxide is 10, and teos solution is made；Its
In, 20 parts by weight of ethyl orthosilicate, 80 parts by weight of deionized water；
B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution made from step a, heats up and stirs
Reaction, reaction temperature are 120 DEG C, time 150min, and then adjusting pH value using acid solution is 6, are cooled down after reaction, instead
It filters again, washing, until the pH value of filtrate is 7, by much filtrate drying and pulverizes, the coated porous calcium phosphate of Silica hydrogel is made
Composite powder；Wherein, 8 parts by weight of graphene, 22 parts by weight of porous calcium phosphate microsphere, 70 parts by weight of teos solution；
C, filtering, dry by the infiltration 2h in organic solvent of composite powder made from step b, further with polymer, dispersing agent
The heat-resisting masterbatch of graphene is made using double screw extruder extruding pelletization in mixing；Wherein, organic solvent is toluene cyclohexanone, is gathered
Conjunction object is polyethylene, and dispersing agent is odium stearate；30 parts by weight of composite powder, 69 parts by weight of polymer, 1 parts by weight of dispersing agent.
Comparative example 1
By graphene powder infiltration, 2.5h, filtering, drying utilize further with polymer, dispersant in organic solvent
The heat-resisting masterbatch of graphene is made in double screw extruder extruding pelletization；Wherein, 35 parts by weight of graphene powder, 63 weight of polymer
Part, 2 parts by weight of dispersing agent, organic solvent is acetone, and polymer is polyethylene, and dispersing agent is zinc stearate.
Graphene masterbatch made from above-described embodiment 1 ~ 5 and comparative example 1 and polyethylene are prepared with mass ratio 1:8 for conveying
The pipeline of hot water carries out heat resistance test referring to GB/T 28799-2012 standard, II type Pipe samples of standard is made, tests
Condition is to be heated to 100 DEG C, and 4.5MPa, time 2000h, the results are shown in Table 1.
Table 1:
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 |
| Long-term quiet leakage scenarios | Ne-leakage | Ne-leakage | Ne-leakage | Ne-leakage | Ne-leakage | 1500h is leaked |
Claims (9)
1. a kind of preparation method of the heat-resisting masterbatch of hot water plastic tube special graphite alkene, it is characterised in that: specific preparation step are as follows:
A, ethyl orthosilicate is dissolved in deionized water, adjusting pH value using ammonium hydroxide is 10, and teos solution is made；
B, the porous calcium phosphate microsphere for loading graphene is immersed in teos solution made from step a, heats up and stirs
Reaction, then adjusting pH value using acid solution is 6 ~ 7, is cooled down after reaction, filters, washs repeatedly, until the pH value of filtrate
It is 7, by much filtrate drying and pulverizes, the coated porous calcium phosphate composite powder of Silica hydrogel is made；
C, filtering, dry by the infiltration 2 ~ 3h in organic solvent of composite powder made from step b, further with polymer, dispersion
The heat-resisting masterbatch of graphene is made using double screw extruder extruding pelletization in agent mixing.
2. the preparation method of the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene according to claim 1, it is characterised in that:
In step a, 20 ~ 30 parts by weight of ethyl orthosilicate, 70 ~ 80 parts by weight of deionized water.
3. the preparation method of the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene according to claim 1, it is characterised in that:
In the step b, 8 ~ 12 parts by weight of graphene, 22 ~ 30 parts by weight of porous calcium phosphate microsphere, 58 ~ 70 weight of teos solution
Measure part.
4. the preparation method of the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene according to claim 1, it is characterised in that:
In the step b, reaction temperature is 120 ~ 150 DEG C, and the time is 90 ~ 150min.
5. the preparation method of the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene according to claim 1, it is characterised in that:
In the step c, organic solvent is acetone, espeleton, methylisobutylketone, cyclohexanone, toluene cyclohexanone, methyl acetate, vinegar
One of acetoacetic ester, propyl acetate, acetonitrile, pyridine.
6. the preparation method of the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene according to claim 1, it is characterised in that:
In the step c, polymer is one of polyethylene, polypropylene.
7. the preparation method of the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene according to claim 1, it is characterised in that:
In the step c, dispersing agent is zinc stearate, in calcium stearate, magnesium stearate, copper stearate, odium stearate, potassium stearate
It is at least one.
8. the preparation method of the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene according to claim 1, it is characterised in that:
In step c, 30 ~ 40 parts by weight of composite powder, 57 ~ 69 parts by weight of polymer, 1 ~ 3 parts by weight of dispersing agent.
9. the heat-resisting masterbatch of a kind of hot water plastic tube special graphite alkene that any one of claim 1 ~ 8 the method is prepared.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113189717A (en) * | 2021-05-12 | 2021-07-30 | 四川天邑康和通信股份有限公司 | Optical fiber of MPO/MTP type connector and preparation method thereof |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113189717A (en) * | 2021-05-12 | 2021-07-30 | 四川天邑康和通信股份有限公司 | Optical fiber of MPO/MTP type connector and preparation method thereof |
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Application publication date: 20190118 |