CN108034297A - A kind of preparation method of mineral coating graphene additive - Google Patents
A kind of preparation method of mineral coating graphene additive Download PDFInfo
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- CN108034297A CN108034297A CN201810079266.8A CN201810079266A CN108034297A CN 108034297 A CN108034297 A CN 108034297A CN 201810079266 A CN201810079266 A CN 201810079266A CN 108034297 A CN108034297 A CN 108034297A
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- carbon source
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- mineral coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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Abstract
A kind of preparation method the invention discloses mineral coating with graphene additive, comprises the following steps that：Biomass carbon source is sent into single screw extrusion machine with pore creating material and is mixed, carries out carbonization treatment, forms the carbon source predecessor with loose structure；After obtained carbon source predecessor is mixed with modification of chitosan solution, high-speed stirred disperses 35 45min under conditions of 60 80 DEG C, 2000 4000r/min, forms chitin modified carbon source dispersed paste.The present invention forms porous carbon source presoma using the biomass carbon source of high temperature cabonization, carbon matrix precursor dispersed paste is obtained by modification of chitosan modification, carbon matrix precursor is peeled off to form graphene using the high shear of microjet nanometer homogenizer, the Quick mechanical for realizing graphene is peeled off, reduce the fault of construction of graphene surface, improve the dispersiveness and lubricity of graphene；The present invention is used in mineral coating as additive, enhances the intensity and water resistance of coating.
Description
Technical field
The present invention relates to additive preparing technical field, is specifically a kind of preparation side of mineral coating graphene additive
Method.
Background technology
With the continuous enhancing of social progress, development in science and technology and people's environmental consciousness, people are to house decoraton
It is required that it is also higher and higher, beautiful beauty is not only needed, more requires environment protection health.However, interior/exterior decoration material on the market is big
Majority is organic material or organic/inorganic composite material, they contain a large amount of volatile organic matters（VOC）, such as formaldehyde, make moist
Afterwards easily colour fading, yellowing, it is mouldy, come off, and there are it is easy to aging the problem of and inflammable security risk.In addition, big fire in recent years
Accident frequently occurs, these all bring huge economic loss, therefore research safety, nontoxic, fire prevention, dress to the country and people
Enrich, good weatherability, building and ornament materials of low cost become research hotspot by effect for decorations, greatly develops such building decoration material
Material is the demand in epoch and the needs of reality.
The content of the invention
It is an object of the invention to provide a kind of mineral coating graphene environmentally protective, security is good, of low cost
The preparation method of additive, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical solution：
A kind of mineral coating preparation method of graphene additive, comprises the following steps that：
（1）The biomass carbon source of 100-120 parts of parts by weight is sent into single screw extrusion machine with the pore creating material of 3-5 parts by weight and is mixed
30-50min is stirred, sets carburizing temperature to form the carbon source forerunner with loose structure for 350-450 DEG C of progress carbonization treatment
Thing；
（2）By modification of chitosan solution that obtained carbon source predecessor and concentration are 11-15mol/L by 1：The mass ratio of 6-8 mixes
After conjunction, high-speed stirred disperses 35-45min under conditions of 60-80 DEG C, 2000-4000r/min, forms chitin modified carbon
Source dispersed paste；
（3）High-pressure fluid is formed by being sent into through chitin modified carbon source dispersed paste in microjet nanometer homogenizer, is set equal
Matter pressure is 110-120Mpa, and by producing huge barometric gradient before and after valve opening, form high speed shear effect makes high-pressure fluid
Carbon source crushes rupture, crushes the carbon source slurry after rupture and high-speed jet is formed after valve opening, is carried out with the jet stream of opposite direction high
The shearing that speed collision reaches carbon source is peeled off, and forms graphene slurry；
（4）150-200 parts of bases are heated to 70-90 DEG C in oily magnetic agitation water-bath heater, add 10-20 parts of boric acid
Ester carries out being sufficiently stirred 20-40min；
（5）Graphene slurry and phosphor-included additive are put into the water-bath heater, and make graphene slurry and phosphorous addition
Agent is scattered at 70-90 DEG C in the base oil；
（6）Dispersant and antioxidant are added, is sufficiently stirred 30-50min so that dispersant and antioxidant are dissolved completely in described
Graphene additive finished product is obtained in base oil.
As the further scheme of the present invention：
The base oil is neopentyl alcohol, one in trimethylolpropane, pentaerythrite, crude palm oil, degreasing lard, coconut oil
Kind, or several homogeneous compositions.
As the further scheme of the present invention：
The dispersant is tween, oleic acid, imine compound, neopelex, hydrogenated styrene-diene copolymer
And the one or more of Span-80.
As the further scheme of the present invention：
The antioxidant selects at least one of shield phenol type antioxidant or amine type antioxidant.
As further scheme of the invention：
The phosphor-included additive selects at least one of organophosphorus ester or acid phosphatase ammonium salt.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention forms porous carbon source presoma using the biomass carbon source of high temperature cabonization, is obtained by modification of chitosan modification
To carbon matrix precursor dispersed paste, carbon matrix precursor is peeled off to form graphene using the high shear of microjet nanometer homogenizer, it is real
The Quick mechanical for having showed graphene is peeled off, and reduces the fault of construction of graphene surface, improves the dispersiveness and profit of graphene
Slip；The present invention is used in mineral coating as additive, enhances the intensity and water resistance of coating.
Embodiment
The technical solution of this patent is described in more detail with reference to embodiment.
Embodiment 1
A kind of mineral coating preparation method of graphene additive, comprises the following steps that：
（1）The pore creating material of the biomass carbon source of 100 parts of parts by weight and 3 parts by weight is sent into single screw extrusion machine and is mixed
30min, sets carburizing temperature to form the carbon source predecessor with loose structure for 350 DEG C of progress carbonization treatments；
（2）By modification of chitosan solution that obtained carbon source predecessor and concentration are 11mol/L by 1：After 6 mass ratio mixing,
High-speed stirred disperses 35min under conditions of 60 DEG C, 2000r/min, forms chitin modified carbon source dispersed paste；
（3）High-pressure fluid is formed by being sent into through chitin modified carbon source dispersed paste in microjet nanometer homogenizer, is set equal
Matter pressure is 110Mpa, and for high-pressure fluid by producing huge barometric gradient before and after valve opening, forming high speed shear effect makes carbon source
Rupture is crushed, the carbon source slurry after rupture is crushed and high-speed jet is formed after valve opening, with the jet stream of opposite direction touch at a high speed
The shearing stripping for reaching carbon source is hit, forms graphene slurry；
（4）150 parts of bases are heated to 70 DEG C in oily magnetic agitation water-bath heater, 10 parts of borates is added and carries out fully
Stir 20min；
（5）Graphene slurry and phosphor-included additive are put into the water-bath heater, and make graphene slurry and phosphorous addition
Agent is scattered at 70 DEG C in the base oil；
（6）Dispersant and antioxidant are added, is sufficiently stirred 30min so that dispersant and antioxidant are dissolved completely in the base
Graphene additive finished product is obtained in plinth oil.
Embodiment 2
A kind of mineral coating preparation method of graphene additive, comprises the following steps that：
（1）The pore creating material of the biomass carbon source of 105 parts of parts by weight and 3.5 parts by weight is sent into single screw extrusion machine and is mixed
35min, sets carburizing temperature to form the carbon source predecessor with loose structure for 380 DEG C of progress carbonization treatments；
（2）By modification of chitosan solution that obtained carbon source predecessor and concentration are 12mol/L by 1：6.5 mass ratio mixing
Afterwards, high-speed stirred disperses 38min under conditions of 65 DEG C, 2500r/min, forms chitin modified carbon source dispersed paste；
（3）High-pressure fluid is formed by being sent into through chitin modified carbon source dispersed paste in microjet nanometer homogenizer, is set equal
Matter pressure is 112Mpa, and for high-pressure fluid by producing huge barometric gradient before and after valve opening, forming high speed shear effect makes carbon source
Rupture is crushed, the carbon source slurry after rupture is crushed and high-speed jet is formed after valve opening, with the jet stream of opposite direction touch at a high speed
The shearing stripping for reaching carbon source is hit, forms graphene slurry；
（4）160 parts of bases are heated to 75 DEG C in oily magnetic agitation water-bath heater, 12 parts of borates is added and carries out fully
Stir 25min；
（5）Graphene slurry and phosphor-included additive are put into the water-bath heater, and make graphene slurry and phosphorous addition
Agent is scattered at 75 DEG C in the base oil；
（6）Dispersant and antioxidant are added, is sufficiently stirred 35min so that dispersant and antioxidant are dissolved completely in the base
Graphene additive finished product is obtained in plinth oil.
Embodiment 3
A kind of mineral coating preparation method of graphene additive, comprises the following steps that：
（1）The pore creating material of the biomass carbon source of 110 parts of parts by weight and 4 parts by weight is sent into single screw extrusion machine and is mixed
40min, sets carburizing temperature to form the carbon source predecessor with loose structure for 400 DEG C of progress carbonization treatments；
（2）By modification of chitosan solution that obtained carbon source predecessor and concentration are 13mol/L by 1：After 7 mass ratio mixing,
High-speed stirred disperses 40min under conditions of 70 DEG C, 3000r/min, forms chitin modified carbon source dispersed paste；
（3）High-pressure fluid is formed by being sent into through chitin modified carbon source dispersed paste in microjet nanometer homogenizer, is set equal
Matter pressure is 115Mpa, and for high-pressure fluid by producing huge barometric gradient before and after valve opening, forming high speed shear effect makes carbon source
Rupture is crushed, the carbon source slurry after rupture is crushed and high-speed jet is formed after valve opening, with the jet stream of opposite direction touch at a high speed
The shearing stripping for reaching carbon source is hit, forms graphene slurry；
（4）180 parts of bases are heated to 80 DEG C in oily magnetic agitation water-bath heater, 15 parts of borates is added and carries out fully
Stir 30min；
（5）Graphene slurry and phosphor-included additive are put into the water-bath heater, and make graphene slurry and phosphorous addition
Agent is scattered at 80 DEG C in the base oil；
（6）Dispersant and antioxidant are added, is sufficiently stirred 40min so that dispersant and antioxidant are dissolved completely in the base
Graphene additive finished product is obtained in plinth oil.
Embodiment 4
A kind of mineral coating preparation method of graphene additive, comprises the following steps that：
（1）The pore creating material of the biomass carbon source of 115 parts of parts by weight and 4.5 parts by weight is sent into single screw extrusion machine and is mixed
45min, sets carburizing temperature to form the carbon source predecessor with loose structure for 420 DEG C of progress carbonization treatments；
（2）By modification of chitosan solution that obtained carbon source predecessor and concentration are 14mol/L by 1：7.5 mass ratio mixing
Afterwards, high-speed stirred disperses 42min under conditions of 75 DEG C, 3500r/min, forms chitin modified carbon source dispersed paste；
（3）High-pressure fluid is formed by being sent into through chitin modified carbon source dispersed paste in microjet nanometer homogenizer, is set equal
Matter pressure is 118Mpa, and for high-pressure fluid by producing huge barometric gradient before and after valve opening, forming high speed shear effect makes carbon source
Rupture is crushed, the carbon source slurry after rupture is crushed and high-speed jet is formed after valve opening, with the jet stream of opposite direction touch at a high speed
The shearing stripping for reaching carbon source is hit, forms graphene slurry；
（4）190 parts of bases are heated to 85 DEG C in oily magnetic agitation water-bath heater, 18 parts of borates is added and carries out fully
Stir 35min；
（5）Graphene slurry and phosphor-included additive are put into the water-bath heater, and make graphene slurry and phosphorous addition
Agent is scattered at 85 DEG C in the base oil；
（6）Dispersant and antioxidant are added, is sufficiently stirred 45min so that dispersant and antioxidant are dissolved completely in the base
Graphene additive finished product is obtained in plinth oil.
Embodiment 5
A kind of mineral coating preparation method of graphene additive, comprises the following steps that：
（1）The pore creating material of the biomass carbon source of 120 parts of parts by weight and 5 parts by weight is sent into single screw extrusion machine and is mixed
50min, sets carburizing temperature to form the carbon source predecessor with loose structure for 450 DEG C of progress carbonization treatments；
（2）By modification of chitosan solution that obtained carbon source predecessor and concentration are 15mol/L by 1：After 8 mass ratio mixing,
High-speed stirred disperses 45min under conditions of 80 DEG C, 4000r/min, forms chitin modified carbon source dispersed paste；
（3）High-pressure fluid is formed by being sent into through chitin modified carbon source dispersed paste in microjet nanometer homogenizer, is set equal
Matter pressure is 120Mpa, and for high-pressure fluid by producing huge barometric gradient before and after valve opening, forming high speed shear effect makes carbon source
Rupture is crushed, the carbon source slurry after rupture is crushed and high-speed jet is formed after valve opening, with the jet stream of opposite direction touch at a high speed
The shearing stripping for reaching carbon source is hit, forms graphene slurry；
（4）200 parts of bases are heated to 90 DEG C in oily magnetic agitation water-bath heater, 20 parts of borates is added and carries out fully
Stir 40min；
（5）Graphene slurry and phosphor-included additive are put into the water-bath heater, and make graphene slurry and phosphorous addition
Agent is scattered at 90 DEG C in the base oil；
（6）Dispersant and antioxidant are added, is sufficiently stirred 50min so that dispersant and antioxidant are dissolved completely in the base
Graphene additive finished product is obtained in plinth oil.
The base oil is neopentyl alcohol, in trimethylolpropane, pentaerythrite, crude palm oil, degreasing lard, coconut oil
One kind, or several homogeneous compositions.The dispersant for tween, oleic acid, imine compound, neopelex,
The one or more of hydrogenated styrene-diene copolymer and Span-80.The antioxidant selects shield phenol type antioxidant or amine type
At least one of antioxidant.The phosphor-included additive selects at least one of organophosphorus ester or acid phosphatase ammonium salt.
The present invention forms porous carbon source presoma using the biomass carbon source of high temperature cabonization, at modification of chitosan modification
Reason obtains carbon matrix precursor dispersed paste, and carbon matrix precursor is peeled off to form graphite using the high shear of microjet nanometer homogenizer
Alkene, the Quick mechanical for realizing graphene are peeled off, and are reduced the fault of construction of graphene surface, are improved the dispersiveness of graphene
And lubricity；The present invention is used in mineral coating as additive, enhances the intensity and water resistance of coating.
The better embodiment of this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
Formula, can also be on the premise of this patent objective not be departed from the knowledge that one skilled in the relevant art possesses
Various changes can be made.
Claims (5)
1. a kind of mineral coating preparation method of graphene additive, it is characterised in that comprise the following steps that：
(1) the biomass carbon source of 100-120 parts of parts by weight is sent into single screw extrusion machine with the pore creating material of 3-5 parts by weight and mixed
30-50min is stirred, sets carburizing temperature to form the carbon source forerunner with loose structure for 350-450 DEG C of progress carbonization treatment
Thing；
(2) by modification of chitosan solution that obtained carbon source predecessor and concentration are 11-15mol/L by 1：The mass ratio of 6-8 mixes
After conjunction, high-speed stirred disperses 35-45min under conditions of 60-80 DEG C, 2000-4000r/min, forms chitin modified carbon
Source dispersed paste；
(3) it will be sent into through chitin modified carbon source dispersed paste in microjet nanometer homogenizer and form high-pressure fluid, set equal
Matter pressure is 110-120Mpa, and by producing huge barometric gradient before and after valve opening, form high speed shear effect makes high-pressure fluid
Carbon source crushes rupture, crushes the carbon source slurry after rupture and high-speed jet is formed after valve opening, is carried out with the jet stream of opposite direction high
The shearing that speed collision reaches carbon source is peeled off, and forms graphene slurry；
(4) 150-200 parts of bases are heated to 70-90 DEG C in oily magnetic agitation water-bath heater, add 10-20 parts of boric acid
Ester carries out being sufficiently stirred 20-40min；
(5) graphene slurry and phosphor-included additive are put into the water-bath heater, and makes graphene slurry and phosphorous addition
Agent is scattered at 70-90 DEG C in the base oil；
(6) dispersant and antioxidant are added, is sufficiently stirred 30-50min so that dispersant and antioxidant are dissolved completely in described
Graphene additive finished product is obtained in base oil.
2. the mineral coating according to claim 1 preparation method of graphene additive, it is characterised in that the basis
Oil is neopentyl alcohol, trimethylolpropane, pentaerythrite, crude palm oil, degreasing lard, a kind of or several equal in coconut oil
Combined thing.
3. the mineral coating according to claim 1 preparation method of graphene additive, it is characterised in that described scattered
Agent is tween, oleic acid, imine compound, neopelex, hydrogenated styrene-diene copolymer and Span-80
It is one or more of.
4. the mineral coating according to claim 1 preparation method of graphene additive, it is characterised in that the antioxygen
At least one of shield phenol type antioxidant or amine type antioxidant are selected in agent.
5. the mineral coating according to claim 1 preparation method of graphene additive, it is characterised in that described phosphorous
Additive selects at least one of organophosphorus ester or acid phosphatase ammonium salt.
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| CN201810079266.8A CN108034297A (en) | 2018-01-26 | 2018-01-26 | A kind of preparation method of mineral coating graphene additive |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127638A (en) * | 2019-06-11 | 2019-08-16 | 上海大学 | A kind of preparation method of nanoscale class graphite-phase two dimension carbonitride dispersion liquid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670737A (en) * | 2016-02-29 | 2016-06-15 | 成都新柯力化工科技有限公司 | Preparation method of graphene lubricating additive |
| CN106590840A (en) * | 2016-12-06 | 2017-04-26 | 重庆中领环保产业技术研究院有限公司 | Lubricating oil additive with doped carbon nano-graphene and preparation method thereof |
| CN106957706A (en) * | 2017-04-17 | 2017-07-18 | 奎克化学（中国）有限公司 | A kind of metal rolling oil containing modified graphene oxide and preparation method thereof |
| CN107325611A (en) * | 2017-06-28 | 2017-11-07 | 安徽慕曼德家具有限公司 | A kind of furniture anticorrosive paint additive |
-
2018
- 2018-01-26 CN CN201810079266.8A patent/CN108034297A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670737A (en) * | 2016-02-29 | 2016-06-15 | 成都新柯力化工科技有限公司 | Preparation method of graphene lubricating additive |
| CN106590840A (en) * | 2016-12-06 | 2017-04-26 | 重庆中领环保产业技术研究院有限公司 | Lubricating oil additive with doped carbon nano-graphene and preparation method thereof |
| CN106957706A (en) * | 2017-04-17 | 2017-07-18 | 奎克化学（中国）有限公司 | A kind of metal rolling oil containing modified graphene oxide and preparation method thereof |
| CN107325611A (en) * | 2017-06-28 | 2017-11-07 | 安徽慕曼德家具有限公司 | A kind of furniture anticorrosive paint additive |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127638A (en) * | 2019-06-11 | 2019-08-16 | 上海大学 | A kind of preparation method of nanoscale class graphite-phase two dimension carbonitride dispersion liquid |
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