CN105778111A - Preparation method and application of novel laminar composite - Google Patents
Preparation method and application of novel laminar composite Download PDFInfo
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- CN105778111A CN105778111A CN201610128416.0A CN201610128416A CN105778111A CN 105778111 A CN105778111 A CN 105778111A CN 201610128416 A CN201610128416 A CN 201610128416A CN 105778111 A CN105778111 A CN 105778111A
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- naphthalene
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- lamellar composite
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses a novel laminar composite.Firstly, polynaphthylene is prepared, polynaphthylene is treated in mixed acid, carboxylated polynaphthylene is obtained, finally the surface of carboxylated polynaphthylene is grafted with polyethylene glycol under a certain condition, and the composite in which polynaphthylene is grafted with polyethylene glycol is obtained.The composite can be hydrolyzed in water, cement can be effectively adsorbed, and diffusion and electric double layers are formed.Due to the fact that cement particles carry the same charge to generate repulsion, the cement particles are diffused, and the composite can be applied to a water reducing agent.The composite is simple in preparation method, good in stability and low in production cost.
Description
Technical field:
The present invention relates to technical field of composite materials, be specifically related to a kind of novel lamellar composite.
Background technology:
Condensed-nuclei aromatics abundance, is present in oil and coal tar in a large number, mainly include naphthalene, anthracene, phenanthrene, pyrene, fluoranthene and etc..The monomer of this kind of abundance, once after generating polymer, present the performance of excellence, also Just because of this, condensed-nuclei aromatics polymer has attracted the concern of numerous researcher in recent years.In condensed-nuclei aromatics polymer, poly-naphthalene is again study the earliest, the most fully and one of the polymer of most application prospect.Carboxylated poly-naphthalene can be dissolved in water, and due to the hydrophilic of the lipophile of main chain and carboxyl, it is an amphipathic molecule, and it can be adsorbed on the surface of cement particle, forms diffusion and even electric layer.Produce due to cement particle band like charges to repel, so that cement particle dispersion.Therefore carboxylated poly-naphthalene can apply to water reducer, but in prior art, the preparation method of poly-naphthalene is complex, and product structure is difficult to control to, and have impact on its water-reducing rate further, thus hindering its practical application.
Summary of the invention:
It is an object of the invention to provide a kind of novel lamellar composite, it can be applicable to water reducer, has higher water-reducing rate, and volume is low, and concrete damage of collapsing is little, good stability, and preparation condition is easily controllable, and production cost is low.
For achieving the above object, the present invention is by the following technical solutions:
A kind of novel lamellar composite, this composite can be applicable to water reducer；
Its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.2-1.5ml/min, start to warm up to 550 DEG C, then adjust heating rate, be warming up to 650 DEG C, and it is incubated 4-5h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip H in the flask equipped with poly-naphthalene2SO4With HNO3Nitration mixture, maintenance system temperature 7-10h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: be sequentially added into carboxylated poly-naphthalene and sulphuric acid prepared by step (2) in polyglycol solution, maintenance system temperature 8-16h, after natural cooling, filter through sand core funnel, use water, washing with alcohol, after being positioned over the dry 16-96h of 45-85 DEG C, obtain poly-naphthalene grafting Polyethylene Glycol composite.
Preferred as technique scheme, in step (1), described gas flow optimized is 1.45ml/min.
Preferred as technique scheme, in step (1), described in the speed that starts to warm up be 4.5 DEG C/min.
Preferred as technique scheme, in step (1), the heating rate after described adjustment is 1 DEG C/min.
Preferred as technique scheme, in step (2), H in nitration mixture2SO4With HNO3Volume ratio be 1-3:1.
Preferred as technique scheme, in step (3), the mass fraction of described sulphuric acid is 98.3%.
Preferred as technique scheme, in step (3), the weight/mass percentage composition of polyglycol solution is 0.01%-1.2%.
Preferred as technique scheme, in step (3), the mass ratio of described Polyethylene Glycol, carboxylated poly-naphthalene and sulphuric acid is 1:4:70-90.
The method have the advantages that
Poly-naphthalene has good layer structure, poly-naphthalene after carboxylated can be dissolved in water, it can adsorb cement in its layer structure, the dispersibility making cement is greatly improved, and the cement surface band like charges of the carboxylated poly-naphthalene of surface adsorption and repel, dispersibility is greatly improved, when but poly-naphthalene outer surface covers cement, cement still can be assembled, the present invention has Polyethylene Glycol at carboxylated poly-naphthalene surface grafting, Polyethylene Glycol can be good absorption cement, composite after grafting can be hydrolyzed in water, the diffusion layer being adsorbed on cement particle surface is thickening, dispersion effect is thick, dispersion effect is good；
This composite good stability, preparation condition is easily controllable, and production cost is low, nontoxic, is conducive to environmental conservation.
Detailed description of the invention:
In order to be better understood from the present invention, the present invention is further described by the examples below, and embodiment is served only for explaining the present invention, and the present invention will not constitute any restriction.
Embodiment 1
A kind of novel lamellar composite, this composite can be applicable to water reducer；Its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 4.5g3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.2ml/min, starting the ramp with 4.5 DEG C/min to 550 DEG C, then adjusting heating rate is 1 DEG C/min, is warming up to 650 DEG C, and it is incubated 4h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip 120mlH in the flask equipped with poly-naphthalene2SO4With 40mlHNO3Nitration mixture, maintenance system temperature 7h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: add the polyglycol solution that preparation of high-purity water mass fraction is 0.01% of 0.01g Polyethylene Glycol and 99.99g in two mouthfuls of flasks of a 250ml, stir to Polyethylene Glycol dissolving, then in these two mouthfuls of flasks, add the carboxylated poly-naphthalene of 0.8g and 70mlH2SO4, install thermometer and condensing tube, be then slowly ramped to 60 DEG C, maintenance system temperature 8h, after natural cooling, filters through sand core funnel, uses water, washing with alcohol, after being positioned over the dry 16h of 45 DEG C, obtain poly-naphthalene grafting Polyethylene Glycol composite.
Embodiment 2
A kind of novel lamellar composite, this composite can be applicable to water reducer；Its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 4.5g3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.5ml/min, starting the ramp with 4.5 DEG C/min to 550 DEG C, then adjusting heating rate is 1 DEG C/min, is warming up to 650 DEG C, and it is incubated 5h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip 120mlH in the flask equipped with poly-naphthalene2SO4With 40mlHNO3Nitration mixture, maintenance system temperature 10h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: add the polyglycol solution that preparation of high-purity water mass fraction is 1.2% of 1.2g Polyethylene Glycol and 98.8g in two mouthfuls of flasks of a 250ml, stir to Polyethylene Glycol dissolving, then in these two mouthfuls of flasks, add the carboxylated poly-naphthalene of 4.8g and 70mlH2SO4, install thermometer and condensing tube, be then slowly ramped to 80 DEG C, maintenance system temperature 16h, after natural cooling, filters through sand core funnel, uses water, washing with alcohol, after being positioned over the dry 96h of 85 DEG C, obtain poly-naphthalene grafting Polyethylene Glycol composite.
Embodiment 3
A kind of novel lamellar composite, this composite can be applicable to water reducer；Its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 4.5g3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.3ml/min, starting the ramp with 4.5 DEG C/min to 550 DEG C, then adjusting heating rate is 1 DEG C/min, is warming up to 650 DEG C, and it is incubated 4.2h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip 120mlH in the flask equipped with poly-naphthalene2SO4With 40mlHNO3Nitration mixture, maintenance system temperature 8h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: add the polyglycol solution that preparation of high-purity water mass fraction is 0.03% of 0.03g Polyethylene Glycol and 99.97g in two mouthfuls of flasks of a 250ml, stir to Polyethylene Glycol dissolving, then in these two mouthfuls of flasks, add the carboxylated poly-naphthalene of 0.12g and 70mlH2SO4, install thermometer and condensing tube, be then slowly ramped to 63 DEG C, maintenance system temperature 10h, after natural cooling, filters through sand core funnel, uses water, washing with alcohol, after being positioned over the dry 26h of 55 DEG C, obtain poly-naphthalene grafting Polyethylene Glycol composite.
Embodiment 4
A kind of novel lamellar composite, this composite can be applicable to water reducer；Its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 4.5g3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.35ml/min, starting the ramp with 4.5 DEG C/min to 550 DEG C, then adjusting heating rate is 1 DEG C/min, is warming up to 650 DEG C, and it is incubated 4.4h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip 120mlH in the flask equipped with poly-naphthalene2SO4With 40mlHNO3Nitration mixture, maintenance system temperature 8h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: add the polyglycol solution that preparation of high-purity water mass fraction is 0.5% of 0.5g Polyethylene Glycol and 99.5g in two mouthfuls of flasks of a 250ml, stir to Polyethylene Glycol dissolving, then in these two mouthfuls of flasks, add the carboxylated poly-naphthalene of 2.0g and 70mlH2SO4, install thermometer and condensing tube, be then slowly ramped to 70 DEG C, maintenance system temperature 12h, after natural cooling, filters through sand core funnel, uses water, washing with alcohol, after being positioned over the dry 36h of 65 DEG C, obtain poly-naphthalene grafting Polyethylene Glycol composite.
Embodiment 5
A kind of novel lamellar composite, this composite can be applicable to water reducer；Its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 4.5g3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.4ml/min, starting the ramp with 4.5 DEG C/min to 550 DEG C, then adjusting heating rate is 1 DEG C/min, is warming up to 650 DEG C, and it is incubated 4.6h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip 120mlH in the flask equipped with poly-naphthalene2SO4With 40mlHNO3Nitration mixture, maintenance system temperature 9h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: add the polyglycol solution that preparation of high-purity water mass fraction is 0.9% of 0.9g Polyethylene Glycol and 99.1g in two mouthfuls of flasks of a 250ml, stir to Polyethylene Glycol dissolving, then in these two mouthfuls of flasks, add the carboxylated poly-naphthalene of 3.6g and 70mlH2SO4, install thermometer and condensing tube, be then slowly ramped to 72 DEG C, maintenance system temperature 14h, after natural cooling, filters through sand core funnel, uses water, washing with alcohol, after being positioned over the dry 56h of 70 DEG C, obtain poly-naphthalene grafting Polyethylene Glycol composite.
Embodiment 6
A kind of novel lamellar composite, this composite can be applicable to water reducer；Its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 4.5g3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.45ml/min, starting the ramp with 4.5 DEG C/min to 550 DEG C, then adjusting heating rate is 1 DEG C/min, is warming up to 650 DEG C, and it is incubated 4.8h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip 120mlH in the flask equipped with poly-naphthalene2SO4With 40mlHNO3Nitration mixture, maintenance system temperature 9.5h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: add the polyglycol solution that preparation of high-purity water mass fraction is 1.1% of 1.1g Polyethylene Glycol and 98.9 in two mouthfuls of flasks of a 250ml, stir to Polyethylene Glycol dissolving, then in these two mouthfuls of flasks, add the carboxylated poly-naphthalene of 4.4g and 70mlH2SO4, install thermometer and condensing tube, be then slowly ramped to 77 DEG C, maintenance system temperature 15h, after natural cooling, filters through sand core funnel, uses water, washing with alcohol, after being positioned over the dry 76h of 80 DEG C, obtain poly-naphthalene grafting Polyethylene Glycol composite.
Claims (8)
1. a novel lamellar composite, it is characterised in that this composite can be applicable to water reducer, and its preparation method comprises the following steps:
(1) preparation of poly-naphthalene: weigh 3,4,9,10-tetracarboxylic acid dianhydride is positioned in porcelain boat, then equipped with 3,4, the porcelain boat of 9,10-tetracarboxylic acid dianhydrides is positioned in electric tube furnace, seals, gas in displacement electric tube furnace 3 times, then a straight-through high-purity Ar, gas flow optimized is at 1.2-1.5ml/min, start to warm up to 550 DEG C, then adjust heating rate, be warming up to 650 DEG C, and it is incubated 4-5h, natural cooling, obtain poly-naphthalene；
(2) preparation of carboxylated poly-naphthalene: drip H in the flask equipped with poly-naphthalene2SO4With HNO3Nitration mixture, maintenance system temperature 7-10h, after natural cooling, through filter, washing, obtain carboxylated poly-naphthalene after drying；
(3) preparation of poly-naphthalene grafting Polyethylene Glycol: be sequentially added into carboxylated poly-naphthalene and sulphuric acid prepared by step (2) in polyglycol solution, maintenance system temperature 8-16h, after natural cooling, filter through sand core funnel, use water, washing with alcohol, after being positioned over the dry 16-96h of 45-85 DEG C, obtain novel lamellar composite.
2. a kind of novel lamellar composite as claimed in claim 1, it is characterised in that in step (1), described gas flow optimized is 1.45ml/min.
3. novel lamellar composite as claimed in claim 1 a kind of, it is characterised in that in step (1), described in the speed that starts to warm up be 4.5 DEG C/min.
4. a kind of novel lamellar composite as claimed in claim 1, it is characterised in that in step (1), the heating rate after described adjustment is 1 DEG C/min.
5. a kind of novel lamellar composite as claimed in claim 1, it is characterised in that in step (2), H in nitration mixture2SO4With HNO3Volume ratio be 1-3:1.
6. a kind of novel lamellar composite as claimed in claim 1, it is characterised in that in step (3), the mass fraction of described sulphuric acid is 98.3%.
7. a kind of novel lamellar composite as claimed in claim 1, it is characterised in that in step (3), the weight/mass percentage composition of polyglycol solution is 0.01%-1.2%.
8. a kind of novel lamellar composite as claimed in claim 1, it is characterised in that in step (3), the mass ratio of described Polyethylene Glycol, carboxylated poly-naphthalene and sulphuric acid is 1:4:70-90.
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| CN201610128416.0A CN105778111A (en) | 2016-03-08 | 2016-03-08 | Preparation method and application of novel laminar composite |
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| CN201610128416.0A CN105778111A (en) | 2016-03-08 | 2016-03-08 | Preparation method and application of novel laminar composite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106467608A (en) * | 2016-10-11 | 2017-03-01 | 浙江大学常州工业技术研究院 | A kind of ylmethoxy Polyethylene Glycol, its preparation method and the graphene dispersion liquid and preparation method thereof based on base Polyethylene Glycol |
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| CN102623676A (en) * | 2012-03-29 | 2012-08-01 | 江西苏克尔新材料有限公司 | Composite material for positive pole of lithium-sulfur battery, and positive pole and battery both made of same |
| CN103011675A (en) * | 2012-12-05 | 2013-04-03 | 中科院广州化学有限公司 | Water-based water-reduction type mortar tackifier, as well as preparation method and application thereof |
| CN103288376A (en) * | 2013-05-13 | 2013-09-11 | 张小博 | Synthesizing and compounding method of polycarboxylate-type high-efficiency water reducing agent |
| CN104119021A (en) * | 2014-06-25 | 2014-10-29 | 芜湖市三兴混凝土外加剂有限公司 | High-efficiency water-reducing agent |
| CN105470514A (en) * | 2015-12-29 | 2016-04-06 | 江西师范大学 | Composite material for lithium-sulfur battery positive electrode, preparation method, and positive electrode and battery prepared from composite material |
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2016
- 2016-03-08 CN CN201610128416.0A patent/CN105778111A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010095389A (en) * | 2008-09-19 | 2010-04-30 | Ube Ind Ltd | Hydraulic composition |
| CN102623676A (en) * | 2012-03-29 | 2012-08-01 | 江西苏克尔新材料有限公司 | Composite material for positive pole of lithium-sulfur battery, and positive pole and battery both made of same |
| CN103011675A (en) * | 2012-12-05 | 2013-04-03 | 中科院广州化学有限公司 | Water-based water-reduction type mortar tackifier, as well as preparation method and application thereof |
| CN103288376A (en) * | 2013-05-13 | 2013-09-11 | 张小博 | Synthesizing and compounding method of polycarboxylate-type high-efficiency water reducing agent |
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| CN105470514A (en) * | 2015-12-29 | 2016-04-06 | 江西师范大学 | Composite material for lithium-sulfur battery positive electrode, preparation method, and positive electrode and battery prepared from composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106467608A (en) * | 2016-10-11 | 2017-03-01 | 浙江大学常州工业技术研究院 | A kind of ylmethoxy Polyethylene Glycol, its preparation method and the graphene dispersion liquid and preparation method thereof based on base Polyethylene Glycol |
| CN106467608B (en) * | 2016-10-11 | 2018-05-01 | 浙江大学常州工业技术研究院 | A kind of ylmethoxy polyethylene glycol, its preparation method and the graphene dispersion liquid and preparation method thereof based on base polyethylene glycol |
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Application publication date: 20160720 |