CN109021226A - A kind of aliphatic water reducing agent and preparation method thereof with space steric effect - Google Patents
A kind of aliphatic water reducing agent and preparation method thereof with space steric effect Download PDFInfo
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- CN109021226A CN109021226A CN201710430376.XA CN201710430376A CN109021226A CN 109021226 A CN109021226 A CN 109021226A CN 201710430376 A CN201710430376 A CN 201710430376A CN 109021226 A CN109021226 A CN 109021226A
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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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
-
- 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
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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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/321—Polymers modified by chemical after-treatment with inorganic compounds
- C08G65/326—Polymers modified by chemical after-treatment with inorganic compounds containing sulfur
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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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
-
- 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
Abstract
The invention belongs to concrete high efficiency water reducing agent technical fields, disclose a kind of aliphatic water reducing agent and preparation method thereof with space steric effect.Preparation method of the present invention first prepares the macromolecular intermediate containing carbonyl, then reacts with sulfonating agent and introduce sulfonic acid group, obtains the aliphatic water reducing agent of pectination molecule structure with formaldehyde condensation.Its simple production process and raw material is easy to get.The aliphatic water reducing agent with space steric effect that the method for the present invention is prepared is the aliphatic water reducing agent of pectination molecule structure, with significant space steric effect, design feature with poly carboxylic acid series water reducer, function of slump protection is good, diminishing dispersion performance is further enhanced.It is applied in concrete, volume is low, its folding in concrete consolidate dosage be 0.2%~0.5% can be obtained excellent diminishing dispersion performance (to calculate on the basis of cementitious material weight), and overcome conventional fat race water-reducing agent slump-loss is big, acetone raw material not environmentally the shortcomings that.
Description
Technical field
The invention belongs to concrete high efficiency water reducing agent technical field, in particular to a kind of fat with space steric effect
Race's water-reducing agent and preparation method thereof.
Background technique
Since ordinary portland cement in 1824 comes out, concrete is widely used.In modernization industry height
In fast development process, concrete becomes the essential head of a large amount of infrastructure constructions with its superior performance and cheap price
Material selection, dam, bridge, highway, railway, tunnel, harbour, harbour, airport, subway, industry and in terms of obtain
Obtain increasingly extensive application.According to the statistics made by the departments concerned, the existing various building gross areas in China are greater than 10,000,000,000 m2, wherein absolutely
It is most of using concrete as main material.It can be seen that concrete industry occupies an important strategic position in China.
With the development of modern science and technology and production, various overlength, superelevation, ultra-large type concrete structures, Yi Ji
The great concrete structure used under harsh environment, as skyscraper, bridge spanning the sea, seabed tunnel, offshore production platform, core are anti-
The construction demand of heap, poisonous and harmful waste handling project etc. is answered to be continuously increased.These concrete engineering construction difficulty are big, use ring
Border is severe, maintenance difficult.Since the 1970s, many industrially developed country are faced with some armored concrete knots
Structure, the infrastructure problem of aging such as bridge especially built in one's early years need to put into huge fund and repair or update.China's structure
Durability of Concrete is also very serious in engineering, and the Ministry of Construction has been organized the 1990s to domestic concrete structure
Investigation, it is found that most of industrial buildings and outdoor structures need overhaul after using 25~30 years, in hazardous medium
Building service life only 15~20 years.It is all these that stern challenge all is proposed to traditional concrete.90 years 20th century
In generation, just the U.S. was put forward for the first time the concept of high performance concrete (HPC), it is desirable that concrete, which has, easily to be poured, consolidates without isolating, height
The features such as intensity and excellent durability.Meet the requirement of high performance concrete, high efficiency water reducing agent have become except cement,
The essential 5th kind of component of concrete except water, sand, stone.There is expert to think, effect of the high efficiency water reducing agent in concrete
It has been more than cement.
High efficiency water reducing agent refers in the case where concrete slump is consistent substantially, can be reduced the additional of water consumption
Agent, water-reducing rate is up to 12% or more.Its basic role is: in the case where not reducing unit consumption of water, improving fresh concrete
Workability, improve mobility；Improve the intensity of maturing.Most common concrete high efficiency water reducing agent is naphthalene system height
Imitate water-reducing agent.The water-reducing rate of the water-reducing agent can greatly improve workability of concrete between 15%~25%, and have significant early
Strong feature all plays an important role to improve concrete strength, save cement, reduce energy consumption etc..But naphthalene system diminishing
Agent also exposes during utilization some itself is difficult to the shortcomings that overcoming.Add the concrete slump of naphthalene series high-efficiency water-reducing agent
Loss is big, and i.e. loss is more than half after placing 0.5h, it is difficult to prepare self-compacting concrete and pump concrete；Concrete water bleeding increases,
Workability is caused to reduce fast, or even the durability of meeting crime of injuries by explosive substances to buildings and goods therein；The primary raw material of naphthalene water reducer --- naphthalene is coking work
The byproduct of industry, in today that environmental consciousness is increasingly reinforced, source is limited by increasing.Therefore it develops novel non-
Naphthalene series high-efficiency water-reducing agent has become one of the hot issue of water-reducing agent research.
Aliphatic water reducing agent is a kind of new and effective water-reducing agent developed in recent years.It is with carbonyl containing compound such as third
Based on ketone, butanone, cyclohexanone etc., hydrophilic sulfonic acid group is introduced by sulfonation, is formed under alkaline condition with formaldehyde condensation
The aliphatic macromolecular chain of certain molecular weight size makes molecule have surface active properties.The water-reducing agent water-reducing rate is up to 20%
More than, good water-retaining property strong to cement adaptability can improve the workability of fresh concrete, be a kind of with certain application prospect
New and effective water-reducing agent.
Foreign countries originate in Europe and U.S.'s well cement tolerance blocking to the research of aliphatic high-efficiency water reducing agent.Modified sulfonation
Keto-aldehyde condensation product is used as well cement tolerance blocking to apply for patent the late 1980s first.External some patents at present
Also start to report with other carbonyls such as acetophenone, diacetone alcohol, acetylacetone,2,4-pentanedione, methyl ethyl ketone, Mesityl oxide etc.
Instead of the research achievement of acetone.The country is then concentrated mainly on for the research of aliphatic water reducing agent improves synthesis technology aspect.Have
Scientific worker's discovery, when the proportion of formaldehyde, acetone and sodium sulfite is 2.2:1:0.7, obtained aliphatic water reducing agent
Water-reducing rate is higher.Separately studies have reported that, the aliphatic high-efficiency water reducing agent stability prepared using secondary process for sulfonation is preferable.When third
It is reacted 3 hours when the molar ratio of ketone, formaldehyde and sodium sulfite is 1:2.0:0.4, reactant concentration is 0.40g/mL, resulting production
Object has good dispersion performance, and the water-reducing rate in concrete reaches 19.5%.
Although domestic and international scientific and technical personnel make earnest efforts always the exploitation of aliphatic high-efficiency water reducing agent, from the point of view of status, research
Focus still concentrate in the improvement of existing synthesis technology, used raw material is also mostly acetone, formaldehyde and sodium sulfite.
And be linear molecule currently with the aliphatic water reducing agent that prior art synthesizes, such Water-reducing Admixtures To Cements particle only has electrostatic
Repulsion effect limits further increasing for diminishing dispersion performance without apparent space steric effect.And linear subtract
Aqua molecule common drawback is that slump retaining is poor, therefore such aliphatic water reducing agent equally exists Control Measures for Concrete Slump in application
Degree loses big problem, it is difficult to meet the requirement of high performance concrete, this also causes the application of the water-reducing agent further to be limited
System.Moreover, acetone raw material receives the strict supervision of country, its use is just limited by increasing.
Based on this, it is necessary to design completely new synthesis technology, provide a kind of while there is significant electrostatic repulsive force and sky
Between steric effect, water-reducing rate is high, function of slump protection is good, and be not related to the novel aliphatic water-reducing agent of acetone.
Summary of the invention
In order to overcome, the above-mentioned function of slump protection of aliphatic water reducing agent in the prior art is poor, concrete slump loss is big, acetone
The unobtainable shortcoming and deficiency of raw material subtract the primary purpose of the present invention is that providing a kind of aliphatic with space steric effect
The preparation method of aqua.
Preparation method of the present invention is that dividing greatly containing carbonyl is prepared in raw material using ethyl acetoacetate, polyethylene glycol monoether
Sub- intermediate, then sulfonation, with formaldehyde condensation obtain aliphatic water reducing agent, simple production process and raw material is easy to get.
Another object of the present invention is to provide the aliphatic water reducing agent with space steric effect of above method preparation.This
Invention water-reducing agent is the aliphatic water reducing agent of pectination molecule structure, and function of slump protection is good, diminishing dispersion performance obtains further
It improves.
The purpose of the present invention is realized by following proposal:
A kind of preparation method of the aliphatic water reducing agent with space steric effect, first prepares among the macromolecular containing carbonyl
Body, then reacted with sulfonating agent and introduce sulfonic acid group, the aliphatic water reducing agent of pectination molecule structure is obtained with formaldehyde condensation.
The macromolecular intermediate containing carbonyl is reacted with polyoxyethylene ether by the displacement of ester ether by ethyl acetoacetate
It arrives.
Ethyl acetoacetate used and the mass ratio of polyoxyethylene ether are preferably 10:100~100:5.
The polyoxyethylene ether can be but be not limited to polyethylene glycol monoether etc..
The macromolecular intermediate containing carbonyl is preferably set with polyethylene glycol monoether by ester ether by ethyl acetoacetate
Reaction is changed to obtain.
The mass ratio of ethyl acetoacetate used and polyethylene glycol monoether is preferably 10:100~100:10.
The macromolecular intermediate containing carbonyl can be specifically prepared by method comprising the following steps: by 10~100
The polyoxyethylene ether mixing of the ethyl acetoacetate of parts by weight, 5~100 parts by weight, 80~110 DEG C of reactions 3 under catalyst action
~4 hours, obtain the macromolecular intermediate containing carbonyl.
Further, the macromolecular intermediate containing carbonyl can be specifically prepared by method comprising the following steps:
The polyethylene glycol monoether of the ethyl acetoacetate of 10~100 parts by weight, 10~100 parts by weight is mixed, 80 under catalyst action
~110 DEG C are reacted 3~4 hours, and the macromolecular intermediate containing carbonyl is obtained.
The catalyst is that conventional use of catalyst is reacted in the displacement of this field ester ether, such as sulfuric acid, sodium hydroxide, vinegar
Sour sodium, solid super-strong acid etc..The amount of used catalyst is catalytic amount.
In preparation method of the present invention, the macromolecular intermediate used containing carbonyl, sulfonating agent, formaldehyde mass ratio be (10~
20): (6~15): (60~100).
The condition reacted with sulfonating agent is preferably 40~70 DEG C and reacts 1~2 hour.
It is described to be preferably 75~95 DEG C with the reaction condition of formaldehyde condensation and react 3~4 hours.
The sulfonating agent be sulfonating agent commonly used in the art, such as can for sodium sulfite, sodium hydrogensulfite or
Sodium pyrosulfite.
Preparation method of the present invention carries out in aqueous systems, matter of the amount of water used preferably with the macromolecular intermediate containing carbonyl
Amount is than being 20:20~30:10.
Preparation method of the present invention carries out in alkaline system, the amount of alkali used preferably with the macromolecular intermediate containing carbonyl
Mass ratio is 2:20~3:10.Alkali used is preferably sodium hydroxide.
Specifically, preparation method of the present invention is the following steps are included: first prepare the macromolecular intermediate containing carbonyl, then by 10~
The macromolecular intermediate of 20 parts by weight, the sulfonating agent of 6~15 parts by weight, the alkali of 2~3 parts by weight, the water of 20~30 parts by weight are mixed
It closes, 40~70 DEG C are reacted 1~2 hour；The formalin of 60~100 parts by weight is added, 75~95 DEG C obtain for reaction 3~4 hours
To product.
More specifically, preparation method of the present invention is the following steps are included: by the ethyl acetoacetate of 10~100 parts by weight, 10
The polyethylene glycol monoether of~100 parts by weight mixes, and reacts 3~4 hours for 80~110 DEG C, is obtained containing carbonyl under catalyst action
Macromolecular intermediate；Again by the macromolecular intermediate of 10~20 parts by weight, the sulfonating agents of 6~15 parts by weight, 2~3 parts by weight
The water mixing of alkali, 20~30 parts by weight, 40~70 DEG C are reacted 1~2 hour；Add the formalin of 60~100 parts by weight, 75
~95 DEG C of reactions obtain product in 3~4 hours.
The formalin preferably passes through dropwise addition and is added.
The aliphatic water reducing agent with space steric effect that the method for the present invention is prepared, molecular structure are pectination point
Minor structure has significant space steric effect, the design feature with poly carboxylic acid series water reducer, diminishing good dispersion property,
Concrete slump loss is small.
There is the aliphatic water reducing agent of space steric effect to be applied in concrete the present invention, volume is low, in coagulation
It is that 0.2%~0.5% (being calculated on the basis of cementitious material weight) can be obtained excellent diminishing dispersion that folding in soil, which consolidates dosage,
Performance, and overcome conventional fat race water-reducing agent slump-loss is big, acetone raw material not environmentally the shortcomings that.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
The aliphatic water reducing agent with space steric effect that the present invention synthesizes, water-reducing rate is up to 20~35%；Slump retaining
Can be good, preparation of the concrete slump in 1~2 hour internal loss very little, suitable for high performance concrete；The adaptation of product
By force, good with Multiple Type cement compatibility；Properties of product are stablized；Method is simple, of less demanding to production equipment, is easy to industrialize
Production.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Material involved in the following example can be obtained from commercial channel.
Embodiment 1
50 grams of ethyl acetoacetates, 30 grams of polyethylene glycol monoethers and 2 grams of sodium hydroxides are put into back flow reaction device first
In, 90 DEG C are warming up to, is reacted 3 hours, the macromolecular intermediate containing carbonyl is made.
Macromolecular intermediate made from 20 grams of above-mentioned steps, 10 grams of sodium sulfites, 60 grams of water reflux unit has been put into
Three-necked flask in, adjust pH and be equal to 10, be warming up to 50 DEG C, react 1 hour.Then it is molten to start to be added dropwise 120 gram 37% of formaldehyde
Liquid controls temperature.System is to slowly warm up to 95 DEG C again after formaldehyde is added dropwise, insulation reaction 4 hours, is finally produced
Product.
Embodiment 2
50 grams of ethyl acetoacetates, 30 grams of polyethylene glycol monoethers and 2 grams of sodium hydroxides are put into back flow reaction device first
In, 90 DEG C are warming up to, is reacted 3 hours, the macromolecular intermediate containing carbonyl is made.
Macromolecular intermediate made from 20 grams of above-mentioned steps, 12 grams of sodium sulfites, 60 grams of water reflux unit has been put into
Three-necked flask in, adjust pH and be equal to 10, be warming up to 50 DEG C, react 2 hours.Then it is molten to start to be added dropwise 120 gram 37% of formaldehyde
Liquid controls temperature.System is to slowly warm up to 95 DEG C again after formaldehyde is added dropwise, insulation reaction 4 hours, is finally produced
Product.
Embodiment 3
First by 50 grams of ethyl acetoacetates, 30 grams of polyethylene glycol monoethers and 2 grams of sulfuric acid investment back flow reaction devices, rise
Temperature is reacted 3 hours to 90 DEG C, adjusts pH to neutrality, the macromolecular intermediate containing carbonyl is made.
Macromolecular intermediate made from 20 grams of above-mentioned steps, 10 grams of sodium sulfites, 60 grams of water reflux unit has been put into
Three-necked flask in, adjust pH and be equal to 10, be warming up to 50 DEG C, react 1 hour.Then it is molten to start to be added dropwise 120 gram 37% of formaldehyde
Liquid controls temperature.System is to slowly warm up to 95 DEG C again after formaldehyde is added dropwise, insulation reaction 4 hours, is finally produced
Product.
Embodiment 4
First by 50 grams of ethyl acetoacetates, 30 grams of polyethylene glycol monoethers and 2 grams of sulfuric acid investment back flow reaction devices, rise
Temperature is reacted 3 hours to 90 DEG C, adjusts pH to neutrality, the macromolecular intermediate containing carbonyl is made.
Macromolecular intermediate made from 20 grams of above-mentioned steps, 10 grams of sodium sulfites, 60 grams of water reflux unit has been put into
Three-necked flask in, adjust pH and be equal to 10, be warming up to 50 DEG C, react 1 hour.Then it is molten to start to be added dropwise 120 gram 37% of formaldehyde
Liquid controls temperature.System is to slowly warm up to 80 DEG C again after formaldehyde is added dropwise, insulation reaction 3 hours, is finally produced
Product.
Application experiment of the novel aliphatic high efficiency water reducing agent being prepared the following are Examples 1 to 4 in cement paste
As a result, being specifically shown in Table 1.It can be seen from the data in the table that novel aliphatic water-reducing agent of the invention has stronger diminishing dispersion performance,
When volume is 0.35%, the naphthalene series high-efficiency water-reducing agent that volume is 0.50% is alreadyd exceed to the dispersion performance of cement paste.1
After hour, the cement paste for mixing novel aliphatic high efficiency water reducing agent has still maintained higher mobile performance, and fluidity loss is equal
Less than 10mm；And the flowing degree of net paste of cement loss for mixing 0.50% naphthalene series high-efficiency water-reducing agent and common fats race water-reducing agent reaches
30~40mm, this illustrates that novel aliphatic water-reducing agent of the invention has stronger function of slump protection, this is because its molecule knot
Structure is pectination molecule structure, has side chain, it is possible to provide the steric hindrance of some strength, therefore this is a kind of with brand new
Aliphatic high-efficiency water reducing agent.
Dispersion performance of the 1 novel aliphatic high efficiency water reducing agent of table to cement paste
| Water-reducing agent | Volume；% | Paste flowing degree；mm | Paste flowing degree after 1 hour；mm |
| Naphthalene series high-efficiency water-reducing agent | 0.50 | 150 | 115 |
| Commercially available aliphatic water reducing agent | 0.50 | 155 | 113 |
| Embodiment 1 | 0.35 | 170 | 168 |
| Embodiment 2 | 0.35 | 175 | 171 |
| Embodiment 3 | 0.35 | 162 | 152 |
| Embodiment 4 | 0.35 | 155 | 150 |
(the ratio of mud: 0.28；Cement: Guangdong show board R32.5 ordinary portland cement；The measurement of flowing degree of net paste of cement according to
Chinese national standard GB/T8077-2000 " concrete admixture homogeneity test method " is carried out).
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the aliphatic water reducing agent with space steric effect, it is characterised in that first prepare containing the big of carbonyl
Molecule intermediate, then reacted with sulfonating agent and introduce sulfonic acid group, the aliphatic diminishing of pectination molecule structure is obtained with formaldehyde condensation
Agent.
2. the preparation method of the aliphatic water reducing agent according to claim 1 with space steric effect, it is characterised in that:
The macromolecular intermediate containing carbonyl is reacted to obtain with polyoxyethylene ether by ethyl acetoacetate by the displacement of ester ether；Second used
Ethyl acetoacetic acid ethyl ester and the mass ratio of polyoxyethylene ether are 10:100~100:5.
3. the preparation method of the aliphatic water reducing agent according to claim 2 with space steric effect, it is characterised in that:
The polyoxyethylene ether is polyethylene glycol monoether.
4. the preparation method of the aliphatic water reducing agent according to claim 3 with space steric effect, it is characterised in that:
The macromolecular intermediate containing carbonyl is reacted to obtain with polyethylene glycol monoether by ethyl acetoacetate by the displacement of ester ether；It is used
The mass ratio of ethyl acetoacetate and polyethylene glycol monoether is 10:100~100:10.
5. the preparation method of the aliphatic water reducing agent according to claim 1 with space steric effect, it is characterised in that:
The macromolecular intermediate containing carbonyl is specifically prepared by method comprising the following steps: by the second of 10~100 parts by weight
The polyoxyethylene ether mixing of ethyl acetoacetic acid ethyl ester, 5~100 parts by weight, reacts 3~4 hours for 80~110 DEG C under catalyst action, obtains
To the macromolecular intermediate containing carbonyl.
6. the preparation method of the aliphatic water reducing agent according to claim 4 with space steric effect, it is characterised in that:
The macromolecular intermediate containing carbonyl is specifically prepared by method comprising the following steps: by the second of 10~100 parts by weight
The polyethylene glycol monoether mixing of ethyl acetoacetic acid ethyl ester, 10~100 parts by weight, reacts 3~4 hours for 80~110 DEG C under catalyst action,
Obtain the macromolecular intermediate containing carbonyl.
7. the preparation method of the aliphatic water reducing agent according to claim 1 with space steric effect, it is characterised in that:
Macromolecular intermediate used containing carbonyl, sulfonating agent, formaldehyde mass ratio be (10~20): (6~15): (60~100)；It is described
The condition reacted with sulfonating agent is 40~70 DEG C and reacts 1~2 hour；The reaction condition with formaldehyde condensation is 75~95 DEG C anti-
It answers 3~4 hours.
8. the preparation method of the aliphatic water reducing agent according to claim 1 with space steric effect, it is characterised in that
The following steps are included: first prepare the macromolecular intermediate containing carbonyl, then by the macromolecular intermediate of 10~20 parts by weight, 6~15
The water mixing of the sulfonating agent of parts by weight, the alkali of 2~3 parts by weight, 20~30 parts by weight, 40~70 DEG C are reacted 1~2 hour；Again plus
Enter the formalin of 60~100 parts by weight, 75~95 DEG C of reactions obtain product in 3~4 hours.
9. the preparation method of the aliphatic water reducing agent according to claim 4 with space steric effect, it is characterised in that
The following steps are included: the polyethylene glycol monoether of the ethyl acetoacetate of 10~100 parts by weight, 10~100 parts by weight is mixed, urge
Lower 80~110 DEG C of agent effect are reacted 3~4 hours, and the macromolecular intermediate containing carbonyl is obtained；Again by the big of 10~20 parts by weight
The water mixing of molecule intermediate, the sulfonating agent of 6~15 parts by weight, the alkali of 2~3 parts by weight, 20~30 parts by weight, 40~70 DEG C anti-
It answers 1~2 hour；The formalin of 60~100 parts by weight is added, 75~95 DEG C of reactions obtain product in 3~4 hours.
10. a kind of aliphatic water reducing agent with space steric effect, it is characterised in that any one institute according to claim 1~9
The preparation method stated obtains.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000034151A (en) * | 1998-07-15 | 2000-02-02 | Lion Corp | Cement admixture |
| CN102311548A (en) * | 2011-06-09 | 2012-01-11 | 江苏博特新材料有限公司 | Comb-type lignin water reducer as well as preparation method and application thereof |
| CN103113036A (en) * | 2013-03-12 | 2013-05-22 | 南京瑞迪高新技术有限公司 | Modified aliphatic superplasticizer and preparation method thereof |
| CN104291725A (en) * | 2014-10-10 | 2015-01-21 | 河南科之杰新材料有限公司 | Method for preparing modified aliphatic series water reducing agent |
-
2017
- 2017-06-09 CN CN201710430376.XA patent/CN109021226B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000034151A (en) * | 1998-07-15 | 2000-02-02 | Lion Corp | Cement admixture |
| CN102311548A (en) * | 2011-06-09 | 2012-01-11 | 江苏博特新材料有限公司 | Comb-type lignin water reducer as well as preparation method and application thereof |
| CN103113036A (en) * | 2013-03-12 | 2013-05-22 | 南京瑞迪高新技术有限公司 | Modified aliphatic superplasticizer and preparation method thereof |
| CN104291725A (en) * | 2014-10-10 | 2015-01-21 | 河南科之杰新材料有限公司 | Method for preparing modified aliphatic series water reducing agent |
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