CN110002827A - A kind of aluminate bonding agent of high intensity and preparation method thereof - Google Patents
A kind of aluminate bonding agent of high intensity and preparation method thereof Download PDFInfo
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- CN110002827A CN110002827A CN201910321572.2A CN201910321572A CN110002827A CN 110002827 A CN110002827 A CN 110002827A CN 201910321572 A CN201910321572 A CN 201910321572A CN 110002827 A CN110002827 A CN 110002827A
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- compound
- bonding agent
- added
- aluminate
- aluminate bonding
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/32—Monomers containing only one unsaturated aliphatic radical containing two or more rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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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)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application belongs to chemical field, and in particular to a kind of aluminate bonding agent of high intensity and preparation method thereof.The aluminate bonding agent for high intensity of the application design introduces polyethylene glycol structures in additive and makes it have biggish steric hindrance, effectively aluminate is scatter by the way that additive is added.The early strength function of excited cement is capable of in the addition of additional immunomodulator compounds IV, in cement hydration process, compound IV with and react and generate complex compound soluble easily in water, this is damaged in the impermeable membrane of hyrate and its product such as calcium sulphoaluminate that aquation initial stage can be formed to clinker particle surface, to make rate of dissolution improve, also therefore accelerate with reacting for gypsum, quickening is also added in the generation of calcium sulphoaluminate, and accelerates the conversion rate between sulfate mono salt form calcium sulphoaluminate and entringite obviously.In addition, introducing chlorine atom, its fire protecting performance is effectively increased.
Description
Technical field
The application belongs to chemical field, and in particular to a kind of aluminate bonding agent of high intensity and preparation method thereof.
Background technique
Aluminate cement is mainly used to prepare castable refractory, refractory concrete, fireclay mortar, plays the work of bonding agent
With.From later period the 1950s, refractory concrete has obtained biggish development in China, is widely used in petroleum, chemical industry, builds
It builds, in the industrial departments such as water power, machinery.
The main component of aluminate bonding agent is CA, CA2 and C12A7.Hydration as ambiguity refractory material casting material
Bonding agent, aluminous cement form various calcium aluminate hydrated products and gel aluminum hydroxide by aquation.The CA in hydration process
It is reacted with water and generates CAH10, C2AH8 and aluminium glue, the reaction of CA2 is similar with CA reaction, and the hydration rate of C12A7 is higher.
In the mineral composition of aluminate cement, calcium ion has special importance.I.e. in calcium ion mineral structure
Ligancy is fewer than normal, and irregular, it is easy to generate " cavity ".Calcium aluminate with " cavity " structure just has water
Hardness.After cements water, villous aluminium glue is initially formed around cement granules, with the extension of time, quantity is rapid
Increase.Meanwhile water or hydroxyl ion (O H-) enter in (or penetrating the entrance of aluminium glue film) calcium aluminate mineral structure, then start shape
At drated calcium aluminate.Because aluminium glue package cement granules and plate or needle-shaped drated calcium aluminate interconnect and staggeredly grow, institute
Intensity is obtained with cement setting hardening.In the hydrated product of aluminate cement CAH10, C2AH8 crystallization be capable of forming sheet and
Acicular crystal, takes make friends with mistake mutually, can form firm crystallization connection raw body, and intensity is higher, still, aluminate cement it is long-term
Intensity especially under hygrothermal environment, can be decreased obviously through 1 year~2 years.The reason is that since CAH10, C2AH8 are to be situated between surely
Phase can gradually be transformed into C3AH6 stable phase, this conversion process is spontaneous, and is accelerated due to the raising of temperature.In crystal form
When transformation, a large amount of free water is released, porosity is caused to increase, strength reduction.But intensity decline is not endless, water
The later strength of mudstone declines and reaches minimum, then gos up again.
For these reasons, how to improve CAH10 and C2AH8 into C3AH6 conversion process, under the intensity of aluminous cement
The defect of drop, is a problem to be solved.
Summary of the invention
For the problem that in the prior art, aluminous cement intensity in hydration process declines, and this application provides one kind
New aluminate bonding agent adds compound IV as additive in the aluminate, which has longer alkyl
Chain prays the effect of dispersing agent, in addition, C3A can have been effectively facilitated with the complexing position of cationic bonding by containing on the compound
Conversion rate, the process that CAH10 and C2AH8 are converted to C3AH6 is shortened, to improve the intensity of aluminate bonding agent.
To achieve the goals above, the technological means that the application takes is as follows:
A kind of high-strength aluminate bonding agent contains additional immunomodulator compounds IV, structure in the aluminate bonding agent
Formula is as follows:
The method for preparing high-strength aluminate bonding agent as described in claim 1 is as follows: aluminate bonding agent with it is additional
Agent is uniformly mixed according to mass ratio for 1000~2000:1.
The additional immunomodulator compounds IV's the preparation method is as follows:
The method of the preparation additional immunomodulator compounds, the specific steps are as follows:
(1) raw material 4 is taken, sodium hydroxide is added in 4'- diaminobenzil -2,2'- disulfonic acid, and compound I is made；
(2) raw material A is taken, is passed through 5~15min of nitrogen at room temperature, is warming up to 80~120 DEG C, adipic acid is added, and be passed through
Compound II is made in HCl, insulation reaction 40-60min；
(3) by step (2) prepare compound II be added in reaction kettle, and be passed through pressure 0.2 in nitrogen to kettle~
0.3Mpa is added Na (OH) 2, and is passed through ethylene oxide, maintains the temperature at 120~140 DEG C, reacts 30~50min, obtains compound
III；
(4) compound I, II, III, polymerization inhibitor are added in the reaction vessel, deionized water stirs evenly and is warming up to 100
~160 DEG C, initiator solution is slowly added dropwise, drop speed is 0.5~1d/s, is added dropwise, and 3~8h of insulation reaction stops heating,
It is cooled to room temperature reactant, the extraction of the third ethyl alcohol is added, is spin-dried for solvent, ethyl alcohol recrystallization obtains final product IV.
The molar ratio of compound A and HCl described in step (2) are 1:1~1.25；
The quality of ethanedioic acid described in step (2) is the 10~15% of compound A mass；
The molar ratio of ethylene oxide described in step (3) and compound I are 1:1~1.5；
Initiator described in step (4) is selected from potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate；
The molar ratio of compound I, II, III described in step (4) are 1:1.2~2:0.8~1；
About innovative point of the invention, can be illustrated by following aspects:
The aluminate bonding agent for high intensity of the application design is introduced poly- by the way that additive is added in additive
Ethylene glycol structure makes it have biggish steric hindrance, effectively aluminate is scatter.The addition energy of additional immunomodulator compounds IV
The early strength function of enough excited cements, in cement hydration process, compound IV with and react generation complex compound soluble easily in water, this
It is damaged in the impermeable membrane of hyrate and its product such as calcium sulphoaluminate that aquation initial stage can be formed to clinker particle surface,
To make rate of dissolution improve, also therefore accelerate with reacting for gypsum, quickening is also added in the generation of calcium sulphoaluminate, and makes single sulphur
Conversion rate between hydrochlorate type calcium sulphoaluminate and entringite is obviously accelerated.In addition, introducing chlorine atom, its fire prevention is effectively increased
Performance.
Specific embodiment
Embodiment one
(1) raw material 4 is taken, sodium hydroxide is added in 4'- diaminobenzil -2,2'- disulfonic acid, and compound I is made；
(2) raw material A is taken, is passed through 5~15min of nitrogen at room temperature, is warming up to 80~120 DEG C, adipic acid is added, and be passed through
Compound II is made in HCl, insulation reaction 40-60min, and the molar ratio of compound A and HCl are 1:1, and the quality of ethanedioic acid is to change
Close the 10% of object A mass；
(3) compound II prepared by step (2) is added in reaction kettle, and is passed through pressure in nitrogen to kettle
0.2Mpa is added Na (OH) 2, and is passed through ethylene oxide, maintains the temperature at 120 DEG C, reacts 30min, obtains compound III, described
Ethylene oxide and compound I molar ratio be 1:1；
(4) compound I, II, III, polymerization inhibitor are added in the reaction vessel, deionized water stirs evenly and is warming up to 160
DEG C, initiator solution is slowly added dropwise, drop speed is 0.5d/s, is added dropwise, and insulation reaction 3h stops heating, keeps reactant cooling
To room temperature, the extraction of the third ethyl alcohol is added, is spin-dried for solvent, ethyl alcohol recrystallization obtains final product IV, mole of compound I, II, III
Than for 1:1.2:0.8；The initiator is selected from potassium peroxydisulfate.
Embodiment two
(1) raw material 4 is taken, sodium hydroxide is added in 4'- diaminobenzil -2,2'- disulfonic acid, and compound I is made；
(2) raw material A is taken, is passed through nitrogen 15min at room temperature, is warming up to 120 DEG C, adipic acid is added, and be passed through HCl, is protected
Compound II is made in temperature reaction 60min, and the molar ratio of compound A and HCl are 1:1.25, and the quality of ethanedioic acid is compound A matter
The 15% of amount；
(3) compound II prepared by step (2) is added in reaction kettle, and is passed through pressure in nitrogen to kettle
0.3Mpa is added Na (OH) 2, and is passed through ethylene oxide, maintains the temperature at 120~140 DEG C, reacts 50min, obtains compound III,
The molar ratio of the ethylene oxide and compound I is 1:1；
(4) compound I, II, III, polymerization inhibitor are added in the reaction vessel, deionized water stirs evenly and is warming up to 100
DEG C, initiator solution is slowly added dropwise, drop speed is 0.5~1d/s, is added dropwise, and insulation reaction 8h stops heating, makes reactant
It is cooled to room temperature, the extraction of the third ethyl alcohol is added, is spin-dried for solvent, ethyl alcohol recrystallization obtains final product IV, compound I, II, III's
Molar ratio is 1:2:1；The initiator is selected from ammonium persulfate.
Embodiment three
(1) raw material 4 is taken, sodium hydroxide is added in 4'- diaminobenzil -2,2'- disulfonic acid, and compound I is made；
(2) raw material A is taken, is passed through nitrogen 12min at room temperature, is warming up to 100 DEG C, adipic acid is added, and be passed through HCl, is protected
Compound II is made in temperature reaction 50min, and the molar ratio of compound A and HCl are 1:1.2, and the quality of ethanedioic acid is compound A matter
The 13% of amount；
(3) compound II prepared by step (2) is added in reaction kettle, and is passed through pressure in nitrogen to kettle
0.25Mpa is added Na (OH) 2, and is passed through ethylene oxide, maintains the temperature at 130 DEG C, reacts 45min, obtains compound III, described
Ethylene oxide and compound I molar ratio be 1:1.2；
(4) compound I, II, III, polymerization inhibitor are added in the reaction vessel, deionized water stirs evenly and is warming up to 130
DEG C, initiator solution is slowly added dropwise, drop speed is 0.5~1d/s, is added dropwise, and insulation reaction 6h stops heating, makes reactant
It is cooled to room temperature, the extraction of the third ethyl alcohol is added, is spin-dried for solvent, ethyl alcohol recrystallization obtains final product IV, compound I, II, III's
Molar ratio is 1:1.5:0.9；The initiator is selected from potassium peroxydisulfate.
Claims (8)
1. a kind of high-strength aluminate bonding agent, which is characterized in that contain additional immunomodulator compounds in the aluminate bonding agent
IV, structural formula are as follows:
2. the method for preparing high-strength aluminate bonding agent as described in claim 1 is as follows: it is characterized in that,
The additional immunomodulator compounds IV's the preparation method is as follows:
3. the method for preparing high-strength aluminate bonding agent as claimed in claim 2, which is characterized in that additional described in preparing
The method of immunomodulator compounds, the specific steps are as follows:
(1) raw material 4 is taken, sodium hydroxide is added in 4'- diaminobenzil -2,2'- disulfonic acid, and compound I is made；
(2) raw material A is taken, is passed through 5~15min of nitrogen at room temperature, is warming up to 80~120 DEG C, adipic acid is added, and be passed through HCl,
Compound II is made in insulation reaction 40-60min；
(3) by step (2) prepare compound II be added in reaction kettle, and be passed through pressure 0.2 in nitrogen to kettle~
0.3Mpa is added Na (OH) 2, and is passed through ethylene oxide, maintains the temperature at 120~140 DEG C, reacts 30~50min, obtains compound
III；
(4) it is added compound I, II, III in the reaction vessel, polymerization inhibitor, deionized water, stir evenly and it is warming up to 100~
160 DEG C, initiator solution is slowly added dropwise, drop speed is 0.5~1d/s, is added dropwise, and 3~8h of insulation reaction stops heating, is made
Reactant is cooled to room temperature, and the extraction of the third ethyl alcohol is added, is spin-dried for solvent, ethyl alcohol recrystallization obtains final product IV.
4. the method for preparing high-strength aluminate bonding agent as claimed in claim 3, which is characterized in that described in step (2)
Compound A and HCl molar ratio be 1:1~1.25.
5. the method for preparing high-strength aluminate bonding agent as claimed in claim 3, which is characterized in that described in step (2)
Ethanedioic acid quality be compound A mass 10~15%.
6. the method for preparing high-strength aluminate bonding agent as claimed in claim 3, which is characterized in that described in step (3)
Ethylene oxide and compound I molar ratio be 1:1~1.5.
7. the method for preparing high-strength aluminate bonding agent as claimed in claim 3, which is characterized in that described in step (4)
Initiator be selected from potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate.
8. the method for preparing high-strength aluminate bonding agent as claimed in claim 3, which is characterized in that described in step (4)
Compound I, II, III molar ratio be 1:1.2~2:0.8~1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910321572.2A CN110002827A (en) | 2019-04-22 | 2019-04-22 | A kind of aluminate bonding agent of high intensity and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910321572.2A CN110002827A (en) | 2019-04-22 | 2019-04-22 | A kind of aluminate bonding agent of high intensity and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2033367A (en) * | 1978-11-07 | 1980-05-21 | Coal Industry Patents Ltd | Quick Setting Cements |
| US4357167A (en) * | 1979-09-07 | 1982-11-02 | Coal Industry (Patents) Limited | Methods of stowing cavities with flowable materials |
| EP1004556B1 (en) * | 1998-11-25 | 2001-06-13 | Dyckerhoff Aktiengesellschaft | Hydraulic binder composition and its use |
| CN102770390A (en) * | 2010-02-25 | 2012-11-07 | 建筑研究和技术有限公司 | Hardening accelerator composition containing dispersants |
| CN105934417A (en) * | 2014-01-21 | 2016-09-07 | 巴斯夫欧洲公司 | Calcium sulfate composition comprising an additive |
-
2019
- 2019-04-22 CN CN201910321572.2A patent/CN110002827A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2033367A (en) * | 1978-11-07 | 1980-05-21 | Coal Industry Patents Ltd | Quick Setting Cements |
| US4357167A (en) * | 1979-09-07 | 1982-11-02 | Coal Industry (Patents) Limited | Methods of stowing cavities with flowable materials |
| EP1004556B1 (en) * | 1998-11-25 | 2001-06-13 | Dyckerhoff Aktiengesellschaft | Hydraulic binder composition and its use |
| CN102770390A (en) * | 2010-02-25 | 2012-11-07 | 建筑研究和技术有限公司 | Hardening accelerator composition containing dispersants |
| CN105934417A (en) * | 2014-01-21 | 2016-09-07 | 巴斯夫欧洲公司 | Calcium sulfate composition comprising an additive |
Non-Patent Citations (2)
| Title |
|---|
| 蔡素德: "《有机化学》", 31 July 1989, 中国建筑工业出版社 * |
| 陈冠荣: "《化工百科全书 第7卷 核能技术——计算机技术》", 30 September 1994, 化学工业出版社 * |
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Application publication date: 20190712 |
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