CN106045362A - Alcohol amine early strength agents as well as preparation method and application thereof - Google Patents
Alcohol amine early strength agents as well as preparation method and application thereof Download PDFInfo
- Publication number
- CN106045362A CN106045362A CN201610392181.6A CN201610392181A CN106045362A CN 106045362 A CN106045362 A CN 106045362A CN 201610392181 A CN201610392181 A CN 201610392181A CN 106045362 A CN106045362 A CN 106045362A
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- CN
- China
- Prior art keywords
- early strength
- strength agent
- preparation
- alcamines
- diethanolamine
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Classifications
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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
- C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
- C04B24/122—Hydroxy amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
-
- 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
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses alcohol amine early strength agents as well as a preparation method and an application thereof. The main component of the alcohol amine early strength agents is diethanol mono-propylene glycol amine, and the molecular structure of diethanol mono-propylene glycol amine is shown as the formula (I). The alcohol amine early strength agents are prepared from diethanolamine and glycidol through a reaction in a solvent, the preparation method is simple, conditions are mild, and separation treatment is not needed. The alcohol amine early strength agents have excellent early strength performance and have good compatibility with a polycarboxylate superplasticizer and an inorganic salt early strength agent; the early strength performance of the alcohol amine early strength agents is better than that of commonly used alcohol amine early strength agents such as triethanolamine, N,N-bis(2-hydroxyethyl)isopropanolamine and the like.
Description
Technical field
The present invention relates to cement/technical field of concrete additives, more particularly, to a kind of alcamines early strength agent and
Preparation method and application.
Background technology
Cement/concrete early strength agent is that a class can be accelerated hydrated cementitious speed, promote cement/early age strength of concrete development
Additive.In many cement/concrete workses such as prefabricated components and steam-curing concrete, road and bridge and renovation reinforcement thereof,
The application of early strength agent is significant.For prefabricated components and steam-curing concrete, early strength agent is used can significantly to shorten production week
Phase, improve production efficiency；Road and bridge and renovation reinforcement engineering in apply early strength agent can the reduction of erection time, make road and bridge
Can be the most open-minded, bring significant economic benefit and social benefit.
Conventional early strength agent includes inorganic and organic two big classes.(1) inorganic early strength agent includes strong electrolyte inorganic salt and
A little alkaline inorganic compound, such as sulfate, nitrate, nitrite, alkali metal hydroxide, alkali carbonate, alkali
Metal silicate, alkali metal and alkaline-earth halide etc., the general large usage quantity of mineral-type early strength agent, it is also possible to affect concrete
Later strength and durability；(2) organic early strength agent includes organic alcohol amine, carbamide and carboxylate etc., wherein Organic Alcohol amine
Early strength agent is the most concerned, compared with inorganic early strength agent, consumption few (usual consumption be cement ten thousand/several), adaptive temperature scope
Wide (all can play early strength function from-5 DEG C～90 DEG C), corrosion-free on reinforcing bar, do not affect later strength.
Most currently used Organic Alcohol amine early strength agent includes triethanolamine, triisopropanolamine, diethanol list isopropanol
The addition compound product etc. of amine and ethylenediamine and oxirane.
Summary of the invention
The technical problem to be solved in the present invention is the technology making up the not enough especially Organic Alcohol amine early strength agent of prior art
Not enough, it is provided that a kind of new alcamines early strength agent.Early strength agent containing diethanol MPG amine.
Another technical problem that the invention solves the problems that is to provide the preparation method of described early strength agent.
The present invention also one to solve the technical problem that the application being to provide described early strength agent.
Technical scheme is achieved by the following technical programs:
A kind of alcamines early strength agent is provided, described early strength agent be mainly composed of diethanol MPG amine, described diethyl
The molecular structure of alcohol MPG amine is as shown in formula I:
Present invention simultaneously provides the preparation method of described early strength agent, be to be reacted in a solvent by diethanolamine and epoxy prapanol
And obtain, its fundamental reaction can be schematically as follows:
Specifically, it is that diethanolamine and epoxy prapanol are added in solvent by a certain percentage, maintains the most anti-
After certain time, solvent should be distilled off and i.e. obtain described alcamines early strength agent.
Preferably, described solvent is isopropanol.
Preferably, the ratio (mol ratio) of described diethanolamine and epoxy prapanol is 1～1.2:1.
Preferably, the temperature of described reaction is 40～50 DEG C.
Preferably, the temperature of described reaction is controlled by controlling the rate of addition of epoxy prapanol.
Further, described preparation method comprises the following steps:
S1. diethanolamine and isopropanol are placed in reaction vessel, under stirring condition, dropping epoxy third by a certain percentage
Alcohol, the rate of addition controlling epoxy prapanol makes reaction temperature between 40～50 DEG C；
S2., after epoxy prapanol is added dropwise to complete, 40～50 DEG C of insulation reaction 1～1.5h are continued at；
S3., after step S2 insulation reaction completes, isopropanol solvent is distilled off and obtains described early strength agent.
Preferably, the ratio (mol ratio) of diethanolamine described in step S1 and epoxy prapanol is 1～1.2:1.
Preferably, the temperature of insulation reaction described in step S2 is 50 DEG C, and the time of insulation reaction is 1h.
Present invention simultaneously provides described compound diethanol MPG amine as a kind of new alcamines cement/concrete
The application of early strength agent.
In its application aspect, it strengthens performance and is better than diethanol monoisopropanolamine and triethanolamine, and by itself and polycarboxylic acids
When water reducer and/or inorganic salt early strength agent use in conjunction, there is good suitability.
Beneficial effects of the present invention:
The invention provides a kind of new alcamines early strength agent, there is excellent early strength agent performance.Scientific design of the present invention
The synthetic method of described early strength agent so that the MPG amine Han diethanol in product, except general hydramine in its molecular structure
Outside structure, possibly together with propylene glycol structure, in concrete is applied, this structure has Reduce shrinkage effect, it is possible to reduce concrete curing
During contraction, thus improve concrete strength.When its application is as early strength agent, than existing common hydramine early strength agent
(such as triethanolamine, diethanol monoisopropanolamine etc.) to the raising of concrete strength advantageously.Therefore, present invention simultaneously provides
Described compound diethanol MPG amine is as the application of a kind of new alcamines cement/concrete early strength agent.Further,
In its application aspect, during by diethanol MPG amine with polycarboxylate water-reducer and/or inorganic salt early strength agent use in conjunction, have
Good suitability.
Invention also provides the preparation method of described early strength agent, be successfully obtained a kind of new early strength agent.System of the present invention
Preparation Method is simple to operate, is not related to product separating-purifying, easily realizes.Sum up through lot of experiments, even if containing a small amount of in product
Epoxy prapanol ring opening polymerization product and unreacted diethanolamine, the present invention reaction in produce by-product epoxy prapanol open
Cyclopolymerization product and unreacted diethanolamine have that certain morning is strong or potentiation, it is not necessary to separating-purifying, condition temperature
With, step is clear and definite, and the response time is short, simple.
Detailed description of the invention
The present invention is further illustrated below in conjunction with specific embodiment.Following embodiment being merely cited for property explanation, it is impossible to reason
Solve as limitation of the present invention.Unless stated otherwise, the reagent used in following embodiment obtains for conventional commercial or commercial sources
The reagent obtained, unless stated otherwise, the method and apparatus used in following embodiment is method commonly used in the art and sets
Standby.
Embodiment 1
50mL isopropanol and 21g diethanolamine, under agitation dropping 14.8g epoxy prapanol (two is added in reaction vessel
Ethanolamine and epoxy prapanol mol ratio are 1:1), react for exothermic reaction, control epoxy prapanol rate of addition and make reaction temperature be situated between
In 40～50 DEG C, epoxy prapanol continues to react 1h at 50 DEG C after dripping off, isopropanol solvent is distilled off and obtains product.
Embodiment 2
50mL isopropanol and 25.2g diethanolamine, under agitation dropping 14.8g epoxy prapanol is added in reaction vessel
(diethanolamine with epoxy prapanol mol ratio be 1.2:1), control epoxy prapanol rate of addition make reaction temperature between 40～50 DEG C,
Epoxy prapanol continues to react 1h at 50 DEG C after dripping off, isopropanol solvent is distilled off and obtains product.
Embodiment 3
50mL isopropanol and 23.1g diethanolamine, under agitation dropping 14.8g epoxy prapanol is added in reaction vessel
(diethanolamine with epoxy prapanol mol ratio be 1.1:1), control epoxy prapanol rate of addition make reaction temperature between 40～50 DEG C,
Epoxy prapanol continues to react 1h at 50 DEG C after dripping off, isopropanol solvent is distilled off and obtains product.
Embodiment 4
Detection embodiment 1,2,3 products therefrom understands, products therefrom MPG amine Han diethanol, and its structural formula is:
Product can contain a small amount of epoxy prapanol ring opening polymerization product and unreacted diethanolamine, it is not necessary to point
From.
In order to the advantage of hydramine early strength agent of the present invention is described, by the arbitrary gained early strength agent of the present embodiment 1,2 or 3 with commercially available
Conventional early strength agent diethanol monoisopropanolamine makees glue sand contrast experiment, and glue sand composition and experimental result ask for an interview table 1.
Table 1 embodiment 1,2,3 products therefrom and the glue sand Experimental comparison results of diethanol monoisopropanolamine
* cement: Guangdong show P O 42.5R；* comparative example 1: diethanol monoisopropanolamine
From table 1, early strength agent of the present invention, compared with conventional diethanol monoisopropanolamine, has diminishing merit slightly
Can, the water consumption of preparation similar flow degree mortar is the fewest, and after molding, the comprcssive strength of 3d and 7d is considerably higher, illustrates that the present invention is real
The hydramine early strength agent performance executing example 1 gained is better than diethanol monoisopropanolamine.
Lot of documents is reported, alcamines early strength agent and inorganic salts early strength agent compound use often show cooperative effect, special
Be not with polycarboxylate water-reducer with the use of time, effect is the most notable.In order to investigate early strength agent of the present invention and inorganic salt early strength agent
And the compound use effect of polycarboxylate water-reducer, by the strongest with commercially available conventional hydramine for arbitrary early strength agent in embodiment 1,2,3
Agent triethanolamine is compound with inorganic salt early strength agent potassium bromide and strontium nitrate and polycarboxylate water-reducer respectively makees glue sand contrast experiment,
Glue sand composition and experimental result are shown in Table 2.
Table 2 embodiment 1,2,3 and the glue sand Experimental comparison results of triethanolamine
* cement: Guangdong show P O 42.5R；Water reducer: Dongguan Fu Sheng Industrial Co., Ltd. polycarboxylate water-reducer 2440, dilution
It it is 10% use；* * comparative example 4 complex accelerator: potassium bromide: strontium nitrate: triethanolamine: water=12.5:25:3:160；This
Bright product: potassium bromide: strontium nitrate: the arbitrary example early strength agent of embodiment 1,2,3: water=12.5:25:3:160.
From table 2, compared with triethanolamine (comparative example 4), the Mortar'S Flowability of hydramine early strength agent of the present invention preparation is slightly
Low, but ratio is compared with alone polycarboxylate water-reducer (comparative example 3), and in the case of few 5g water, fluidity is similar；From molding
Blank strength is seen, no matter the mortar strength of the embodiment of the present invention 2 preparation is that the comprcssive strength of 3d or 7d is the highest.Send out for visible
Bright hydramine early strength agent has good suitability with polycarboxylate water-reducer and inorganic salt early strength agent, strengthens performance and is better than three ethanol
Amine.
Claims (10)
1. an alcamines early strength agent, it is characterised in that described early strength agent be mainly composed of diethanol MPG amine, described
The molecular structure of diethanol MPG amine is as shown in formula I:
(I).
2. alcamines early strength agent described in claim 1 is as the application of cement/concrete early strength agent.
3. the preparation method of alcamines early strength agent described in claim 1, it is characterised in that be that diethanolamine and epoxy prapanol are existed
Solvent reacts, solvent is distilled off and get final product.
The preparation method of alcamines early strength agent the most according to claim 3, it is characterised in that described solvent is isopropanol.
The preparation method of alcamines early strength agent the most according to claim 3, it is characterised in that described diethanolamine and epoxy third
The molar ratio of alcohol is 1～1.2:1.
The preparation method of alcamines early strength agent the most according to claim 3, it is characterised in that the temperature of described reaction be 40～
50℃。
The preparation method of alcamines early strength agent the most according to claim 6, it is characterised in that the temperature of described reaction is by control
The rate of addition of epoxy prapanol processed is controlled.
The preparation method of alcamines early strength agent the most according to claim 3, it is characterised in that described preparation method includes following
Step:
S1. diethanolamine and isopropanol are placed in reaction vessel, under stirring condition, drip epoxy prapanol by a certain percentage, control
The rate of addition of epoxy prapanol processed makes reaction temperature between 40～50 DEG C；
S2., after epoxy prapanol is added dropwise to complete, 40～50 DEG C of insulation reaction 1～1.5h are continued at；
S3., after step S2 insulation reaction completes, isopropanol solvent is distilled off and obtains described early strength agent.
The preparation method of alcamines early strength agent the most according to claim 8, it is characterised in that diethanolamine described in step S1 and
The molar ratio of epoxy prapanol is 1～1.2:1；The temperature of insulation reaction described in step S2 is 50 DEG C, and the time of insulation reaction is 1
h。
10. the alcamines early strength agent that preparation method described in any one of claim 3 to 9 prepares is as cement/concrete early
The application of strong agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610392181.6A CN106045362B (en) | 2016-06-02 | 2016-06-02 | A kind of alcamines early strength agent and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610392181.6A CN106045362B (en) | 2016-06-02 | 2016-06-02 | A kind of alcamines early strength agent and its preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106045362A true CN106045362A (en) | 2016-10-26 |
| CN106045362B CN106045362B (en) | 2018-07-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610392181.6A Expired - Fee Related CN106045362B (en) | 2016-06-02 | 2016-06-02 | A kind of alcamines early strength agent and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109592990A (en) * | 2019-02-01 | 2019-04-09 | 马清浩 | A kind of gelling foamed concrete and preparation method thereof |
| CN111646909A (en) * | 2020-04-23 | 2020-09-11 | 安徽海螺新材料科技有限公司 | Preparation method and application of alcohol amine compound capable of improving early strength of cement |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1213656A (en) * | 1998-10-10 | 1999-04-14 | 王宗廷 | Solid hydramine concrete early strength agent |
| CN104311435A (en) * | 2014-09-12 | 2015-01-28 | 北京工业大学 | Polyolamine ester and its synthesis method and use |
-
2016
- 2016-06-02 CN CN201610392181.6A patent/CN106045362B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1213656A (en) * | 1998-10-10 | 1999-04-14 | 王宗廷 | Solid hydramine concrete early strength agent |
| CN104311435A (en) * | 2014-09-12 | 2015-01-28 | 北京工业大学 | Polyolamine ester and its synthesis method and use |
Non-Patent Citations (2)
| Title |
|---|
| TAL SELA ET AL.: "Organic Synthesis "on Water" vs "on Liquids"： A Comparative", 《ORG. LETT.》 * |
| 阮承祥: "《混凝土外加剂及其工程应用》", 31 December 2008, 江西科学技术出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109592990A (en) * | 2019-02-01 | 2019-04-09 | 马清浩 | A kind of gelling foamed concrete and preparation method thereof |
| CN109592990B (en) * | 2019-02-01 | 2021-10-26 | 刘沛灵 | Cementitious foamed concrete and preparation method thereof |
| CN111646909A (en) * | 2020-04-23 | 2020-09-11 | 安徽海螺新材料科技有限公司 | Preparation method and application of alcohol amine compound capable of improving early strength of cement |
| CN111646909B (en) * | 2020-04-23 | 2022-09-06 | 安徽海螺新材料科技有限公司 | Preparation method and application of alcohol amine compound capable of improving early strength of cement |
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| Publication number | Publication date |
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| CN106045362B (en) | 2018-07-31 |
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