CN108659176A - A kind of preparation method of modified polycarboxylic acid water-reducing agent - Google Patents
A kind of preparation method of modified polycarboxylic acid water-reducing agent Download PDFInfo
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- CN108659176A CN108659176A CN201810574944.8A CN201810574944A CN108659176A CN 108659176 A CN108659176 A CN 108659176A CN 201810574944 A CN201810574944 A CN 201810574944A CN 108659176 A CN108659176 A CN 108659176A
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- parts
- water
- reducing agent
- polycarboxylic acid
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- 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
-
- 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
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
- C04B24/2658—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles containing polyether side chains
-
- 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
-
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
-
- 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)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of preparation methods of modified polycarboxylic acid water-reducing agent, include the following steps:0.2 0.5 parts of vitamin C, 25 parts of stabilizer, 30 40 parts of acrylic acid are weighed by weight ratio, puts into dissolve mixing in 30 90 parts of water successively, are expected with obtained A spare；300 400 parts of monomer is placed in 375 600 parts of water and is dissolved, with bottom material is made；Disposably 1/10 A material are put into bottom material, and put into 24 parts of 0.2 0.5 parts of sodium hypophosphite and hydrogen peroxide；Remaining A material are added dropwise immediately, are stirred when being added dropwise；200 400 parts of thionyl chloride is added after keeping the temperature 13 hours and obtains prefabrication the reaction 24 hours of 400 800 parts of sodium azide is added in reaction after 30 90 minutes after；250 480 parts of 2 ethynyl pyridine is added into prefabrication and urges lower dose 25 parts, after neutral alumina desalination after reaction 40min under catalytic action.
Description
Technical field
The present invention relates to building material technical fields, the healthy medicated wine specially made as primary raw material using the deer heart.
Background technology
Polycarboxylate water-reducer is because its volume is low, and water-reducing rate is high, and concrete contraction percentage is low, it is environmentally protective the advantages that and it is extensive
Using.But it is found in concrete production application, the mud in aggregate can adsorb polycarboxylate water-reducer, traditional polycarboxylic acids diminishing
Agent is very sensitive to the clay content in aggregate, with the increase of clay content, the dispersion performance and function of slump protection of polycarboxylate water-reducer
It is substantially reduced, the workability of fresh concrete is caused to decline to a great extent.
Invention content
It is mentioned above in the background art to solve the purpose of the present invention is to provide a kind of modified polycarboxylic acid water-reducing agent
" traditional polycarboxylate water-reducer is very sensitive to the clay content in aggregate, with the increase of clay content, the dispersion of polycarboxylate water-reducer
Performance and function of slump protection are substantially reduced, and the workability of fresh concrete is caused to decline to a great extent " problem.
To achieve the above object, the present invention provides the following technical solutions：
A kind of preparation method of modified polycarboxylic acid water-reducing agent, includes the following steps:
1) 0.2-0.5 parts of vitamin C, 2-5 parts of stabilizer, 30-40 parts of acrylic acid are weighed by weight ratio, are thrown successively
Enter and dissolve mixing in 30-90 parts of water, stir evenly, A material are spare with being made；
2) 300-400 parts of monomer is placed in 375-600 parts of water and is dissolved, and stirred evenly, water temperature is maintained at 5-30 DEG C, matches
Bottom material is made；
3) disposably 1/10 A material are put into bottom material, and puts into 0.2-0.5 parts of sodium hypophosphite and hydrogen peroxide 2-4
Part, it is stirred；
4) remaining A material are added dropwise immediately, are stirred when being added dropwise, 2-3 hour of time for adding, 5-40 DEG C of reaction temperature；
5) 200-400 parts of thionyl chloride is added after keeping the temperature 1-3 hour, sodium azide is added after 30-90 minutes in reaction
After 400-800 parts are reacted 2-4 hours, prefabrication is obtained；
6) 250-480 parts of 2- ethynyl pyridines are added into the prefabrication in step 5) and urge lower dose 2-5 parts, are being catalyzed
After neutral alumina desalination after the lower reaction 40min of effect.
Preferably, the dissolving of monomer is stirred 30-40 minutes after being dissolved in water in step 2), 80-100 revs/min of rotating speed
Clock.
Preferably, the hydrogen peroxide solution that hydrogen peroxide is mass fraction 30-35% in step 3).
Preferably, 2.5 hours of time for adding, 15-25 DEG C of reaction temperature in step 4).
Preferably, the soaking time in step 5) is 1-2 hour.
Preferably, it is CuCl/PMDETA that lower dose is urged described in step 6).
Preferably, the monomer selects allyl alcohol polyethenoxy ether APEG, iso-amylene alcohol ether TPEG, methallyl alcohol
It is one or more in HPEG, acrylic polyoxyethylene ether HPEG, methoxy poly (ethylene glycol) MPEG.
Preferably, the stabilizer is one or more in sodium hydrogensulfite, formaldehyde sodium sulfoxylate, sodium pyrosulfite.
Compared with prior art, the beneficial effects of the invention are as follows：The modified polycarboxylic acid water-reducing agent prepared using the present invention, is subtracted
Water rate is high, and guarantor's effect of collapsing enhances, and reduces to the clay content susceptibility in aggregate, ensure that the workability of fresh concrete.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1：
A kind of preparation method of modified polycarboxylic acid water-reducing agent, includes the following steps:
1) 0.2 part of vitamin C, 2 parts of stabilizer, 30 parts of acrylic acid are weighed by weight ratio, are put into 30 parts of water successively
Dissolving mixing, stirs evenly, and with being made, A material are spare；
2) 300 parts of monomer is placed in 375 parts of water and is dissolved, and stirred evenly, water temperature is maintained at 30 DEG C, with bottom material is made；
3) disposably 1/10 A material are put into bottom material, and put into 3.75 parts of 0.35 part of sodium hypophosphite and hydrogen peroxide,
It is stirred；
4) remaining A material are added dropwise immediately, are stirred when being added dropwise, 2 hours of time for adding, 30 DEG C of reaction temperature；
5) 250 parts of thionyl chloride is added after keeping the temperature 2 hours, 500 parts of reactions 2 of sodium azide are added in reaction after sixty minutes
After hour, prefabrication is obtained；
6) 250 parts of 2- ethynyl pyridines are added into the prefabrication in step 5) and urge lower dose 2 parts, it is anti-under catalytic action
It answers after 40min after neutral alumina desalination.
Alternatively, the dissolving of monomer is stirred 30-40 minutes after being dissolved in water in step 2), rotating speed 80-
100 revs/min.
Alternatively, the hydrogen peroxide solution that hydrogen peroxide is mass fraction 30-35% in step 3).
Alternatively, 2.5 hours of time for adding, 15-25 DEG C of reaction temperature in step 4).
Alternatively, the soaking time in step 5) is 1-2 hour.
Alternatively, it is CuCl/PMDETA that lower dose is urged described in step 6).
Alternatively, the monomer selects allyl alcohol polyethenoxy ether APEG, iso-amylene alcohol ether TPEG, methyl alkene
It is one or more in propyl alcohol HPEG, acrylic polyoxyethylene ether HPEG, methoxy poly (ethylene glycol) MPEG.
Alternatively, the stabilizer is sodium hydrogensulfite, formaldehyde sodium sulfoxylate, one kind in sodium pyrosulfite or more
Kind.
Embodiment one is synthesized to obtained sample, is compared with the aliphatic high-efficiency water reducing agent SAF of the prior art, is used
Standard cement, volume is by cement quality 0.45% (the solid volume of folding), according to GB 8076-2008《Concrete admixture》Efficiently subtract
Aqua detection method surveys its concrete water-reducing ratio and normal pressure bleeding rate ratio.Concrete mix is:Cement 330kg/m3, sand
782kg/m3, stone 1140kg/m3, acquired results are as shown in Table 1：
Table one
The modified polycarboxylic acid water-reducing agent prepared as can be seen from the above table using the present invention, water-reducing rate is high, and guarantor's effect of collapsing increases
By force, air content is high and keep its bleed good, overcomes easy bleeding.
With reference to GB8077-2000《Methods for testing uniformity of concrete admixture》, net slurry is carried out to 1 gained sample of embodiment
Fluidity is tested.W/C is 0.29, and the solid volume of additive folding is the 0.13% of cement consumption, 2.5 grams of bentonites.From following table two
In as can be seen that have obviously to being added to 1 gained sample paste flowing degree of embodiment compared with blank sample (unmodified additive)
Variation illustrates that present invention confrontation mud has obvious effect.
Table two
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition it should be appreciated that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (8)
1. a kind of preparation method of modified polycarboxylic acid water-reducing agent, which is characterized in that include the following steps:
1) 0.2-0.5 parts of vitamin C, 2-5 parts of stabilizer, 30-40 parts of acrylic acid are weighed by weight ratio, put into water successively
Mixing is dissolved in 30-90 parts, is stirred evenly, and with being made, A material are spare；
2) 300-400 parts of monomer is placed in 375-600 parts of water and is dissolved, and stirred evenly, water temperature is maintained at 5-30 DEG C, with being made
Bottom material；
3) disposably 1/10 A material are put into bottom material, and puts into 2-4 parts of 0.2-0.5 parts of sodium hypophosphite and hydrogen peroxide, stirred
Mix mixing；
4) remaining A material are added dropwise immediately, are stirred when being added dropwise, 2-3 hour of time for adding, 5-40 DEG C of reaction temperature；
5) 200-400 parts of thionyl chloride is added after keeping the temperature 1-3 hour, sodium azide 400-800 is added after 30-90 minutes in reaction
After part reaction 2-4 hours, prefabrication is obtained；
6) 250-480 parts of 2- ethynyl pyridines are added into the prefabrication in step 5) and urge lower dose 2-5 parts, under catalytic action
After neutral alumina desalination after reaction 40min.
2. a kind of preparation method of modified polycarboxylic acid water-reducing agent according to claim 1, which is characterized in that single in step 2)
The dissolving of body is stirred 30-40 minutes after being dissolved in water, 80-100 revs/min of rotating speed.
3. a kind of preparation method of modified polycarboxylic acid water-reducing agent according to claim 1, which is characterized in that double in step 3)
Oxygen water is the hydrogen peroxide solution of mass fraction 30-35%.
4. a kind of preparation method of modified polycarboxylic acid water-reducing agent according to claim 1, which is characterized in that drop in step 4)
2.5 hours between added-time, 15-25 DEG C of reaction temperature.
5. a kind of preparation method of modified polycarboxylic acid water-reducing agent according to claim 1, which is characterized in that in step 5)
Soaking time is 1-2 hour.
6. a kind of preparation method of modified polycarboxylic acid water-reducing agent according to claim 1, which is characterized in that institute in step 6)
It is CuCl/PMDETA to state and urge lower dose.
7. a kind of preparation method of modified polycarboxylic acid water-reducing agent according to claim 1-6 any one, which is characterized in that
The monomer selects allyl alcohol polyethenoxy ether APEG, iso-amylene alcohol ether TPEG, methallyl alcohol HPEG, acrylic polyoxyethylene
It is one or more in ether HPEG, methoxy poly (ethylene glycol) MPEG.
8. a kind of preparation method of modified polycarboxylic acid water-reducing agent according to claim 1-6 any one, which is characterized in that
The stabilizer is one or more in sodium hydrogensulfite, formaldehyde sodium sulfoxylate, sodium pyrosulfite.
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| CN201810574944.8A CN108659176A (en) | 2018-06-06 | 2018-06-06 | A kind of preparation method of modified polycarboxylic acid water-reducing agent |
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| CN201810574944.8A CN108659176A (en) | 2018-06-06 | 2018-06-06 | A kind of preparation method of modified polycarboxylic acid water-reducing agent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104945632A (en) * | 2015-06-02 | 2015-09-30 | 江苏奥莱特新材料有限公司 | Preparation method of microspheric polycarboxylic acid water-reducer |
| CN105330834A (en) * | 2015-10-29 | 2016-02-17 | 江苏中铁奥莱特新材料有限公司 | Preparing method for polycarboxylate-type anti-mud water reducer with modified side chain terminal group |
| CN107698717A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of preparation method of anti-mud polycarboxylate water-reducer |
-
2018
- 2018-06-06 CN CN201810574944.8A patent/CN108659176A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104945632A (en) * | 2015-06-02 | 2015-09-30 | 江苏奥莱特新材料有限公司 | Preparation method of microspheric polycarboxylic acid water-reducer |
| CN105330834A (en) * | 2015-10-29 | 2016-02-17 | 江苏中铁奥莱特新材料有限公司 | Preparing method for polycarboxylate-type anti-mud water reducer with modified side chain terminal group |
| CN107698717A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of preparation method of anti-mud polycarboxylate water-reducer |
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Application publication date: 20181016 |