CN106432631B - A kind of polycarboxylate water-reducer and preparation method thereof - Google Patents
A kind of polycarboxylate water-reducer and preparation method thereof Download PDFInfo
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- CN106432631B CN106432631B CN201610846319.5A CN201610846319A CN106432631B CN 106432631 B CN106432631 B CN 106432631B CN 201610846319 A CN201610846319 A CN 201610846319A CN 106432631 B CN106432631 B CN 106432631B
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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
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
Abstract
The present invention provides a kind of polycarboxylate water-reducers, to be prepared by the raw material of following parts by weight through " one kettle way ": 150 parts of modified polyether, 150-280 parts of water, 16-20 parts of acrylic acid, 1-5 parts of ammonium persulfate and 25% reproducibility -5-20 parts of chain-transferring agent solution；Wherein reproducibility-chain-transferring agent is selected from one of more Ammonia dithiocarbonic acid sulfite derivatives shown in formula (I), and the present invention also provides the specific preparation methods of polycarboxylate water-reducer.Polycarboxylate water-reducer provided by the invention, due to replacing traditional reductant Vc and chain-transferring agent thioacetic acid or mercaptopropionic acid using the more Ammonia dithiocarbonic acid sulfite derivatives of reproducibility-chain-transferring agent, it not only can be to avoid the foul smell due to caused by thioacetic acid or mercaptopropionic acid, and toxic action and pollution on the environment of the strong corrosive to human body, and simplify process flow, it can synthesize at normal temperature, improve serious forgiveness.
Description
Technical field
The present invention relates to concrete additive fields, and in particular to a kind of polycarboxylate water-reducer and preparation method thereof.
Background technique
Five kinds of main components of modern concrete are respectively as follows: stone, sand, cement, water and additive.Since additive can be bright
It is aobvious to improve concrete workability, so it becomes essential component in concrete.Polycarboxylate water-reducer is as concrete
Additive is learned, concrete slump can be effectively improved, improves concrete workability, and pollution-free in production process.Nevertheless,
Poly carboxylic acid series water reducer in actual application still there are more technical problems, such as with the adaptability of certain cement it is poor,
Dispersion effect degradation etc. when clay content of gathering materials is higher.
But the advantages such as poly carboxylic acid series water reducer is big with molecular structure adjustability, raw material range of choice is wide, specialize
Just constantly from laboratory, development phase moves towards production application to product.Meanwhile in terms of the production of poly carboxylic acid series water reducer, how into
One step passes through the selection and process modification of raw material, reduces production energy consumption and three waste discharge amounts and industry is generally closed
The hot issue of note.In this regard, the common synthesis temperature of polycarboxylate water-reducer is 50-80 DEG C, but is synthesized at this temperature
Not only it can extend the production time, but also production cost is also relatively high.
The existing room temperature of polycarboxylate water-reducer is prepared at present, and technique is added dropwise, specifically includes the following steps:
Deionization softened water and macromonomer are added in reaction kettle by the first step；
Hydrogen peroxide is added when 75% or more polymeric monomer (modified polyether) dissolution in second step；
Third step starts that A material (thioacetic acid+reductant Vc) is added dropwise, 120min is added dropwise after 10min；
4th step starts that B material (acrylic acid solution) is added dropwise, 110min is added dropwise after 10min；
5th step after being added dropwise to complete, stirs 15min to get the mother liquor of the polycarboxylate water-reducer of solid content 40%.
Poly carboxylic acid series water reducer is a kind of water soluble polymer with pectinate texture, and main chain is usually polyacrylic acid or gathers
Methacrylic acid, the polyethylene glycol of different chain length are side chain.It, can be in polymer molecule by the copolymerization with various function monomers
A variety of functional groups such as carboxyl, sulfonic group, hydroxyl, amido are introduced to realize different application performances；Third is added dropwise in preparation process
Olefin(e) acid solution is the ratio in order to adjust acrylic acid in polymer, and it is the degree of polymerization in order to adjust polymer that thioacetic acid, which is added dropwise,
For the poly carboxylic acid series water reducer of pectinate texture, chain-transferring agent thioacetic acid breath malodor, and chain transfer constant is usually larger,
Cause consumption polymerization reaction early period fast, monomer conversion is difficult to effectively improve.
Above-mentioned dropwise addition reducing agent 120min is the speed in order to control oxidation-reduction reaction, to control initiator generation
Speed, the time for maintaining initiator is long (maintaining 2h), and polymerization reaction, room temperature dropwise addition technique occur under continuous cause
The entire reaction time is 135min, is illustrated in 135min, and the heat that polymerization reaction is released can maintain being normally carried out for reaction.
This reaction is that oxidation-reduction reaction causes system, and the reduzate that oxidant occurs to generate after reduction reaction is chain initiator, such as
The oxidation product that fruit reducing agent occurs to generate after oxidation reaction is just also chain-transferring agent, can thus not have to additional increase chain
Transfer agent thioacetic acid；In addition, if can have a kind of reducing agent, so that the speed of oxidation-reduction reaction slows to 2h or more,
Reducing agent does not just have to be added dropwise in this way, can be added at one time.
Summary of the invention
Based on the above, the present invention develops a kind of new reproducibility-chain-transferring agent, and existed using reproducibility-chain-transferring agent
Method of the room temperature without synthesizing polycarboxylic acid dehydragent under the conditions of dropwise addition, effectively prevents the use of thioacetic acid or mercaptopropionic acid,
And the synthesis technology of simple process, effect stability.
Polycarboxylate water-reducer provided by the invention is to be prepared by the raw material of following parts by weight through " one kettle way ": modified
150 parts of polyethers, 150-280 parts of water, 16-20 parts of acrylic acid, 1-5 parts of ammonium persulfate and 25% reproducibility-chain-transferring agent it is molten
5-20 parts of liquid；
Reproducibility-the chain-transferring agent is selected from more Ammonia dithiocarbonic acid sulfite derivatives shown in formula (I)
One or more of combinations；
In formula (1), R1And R2It is respectively and independently selected from hydrogen bond, substituted or unsubstituted alkylidene, substituted or unsubstituted insatiable hunger
With alkylidene, substituted or unsubstituted cycloalkylidene, substituted or unsubstituted sub- aralkyl, substituted or unsubstituted sub- fragrant oxygen alkane
Base, substituted or unsubstituted aryl and substituted or unsubstituted heteroarylidene；
R3、R4、R5、R6And R7Be respectively and independently selected from hydrogen, substituted or unsubstituted alkyl, substituted or unsubstituted alkenyl,
It is substituted or unsubstituted naphthenic base, substituted or unsubstituted aralkyl, substituted or unsubstituted aralkenyl, substituted or unsubstituted
Aryloxyalkyl group, substituted or unsubstituted aryl, substituted or unsubstituted heteroaryl, substituted or unsubstituted alkyl-carboxylic acid, take
Generation or unsubstituted carboxylate alkyl, substituted or unsubstituted amidoalkyl group, substitution or do not take substituted or unsubstituted ester alkyl
The ketone alkyl in generation and substituted or unsubstituted aldehyde alkyl；
L1 -、L2 -It is identical or different and represent arbitrary SO3 2-、HSO3 -、KSO3 -、NaSO3 -、NH4SO3 -Or R8-SO2 -, and its
In, R8Selected from substituted or unsubstituted alkyl, substituted or unsubstituted alkenyl, substituted or unsubstituted aralkyl and substitution
Or unsubstituted aryl；
N, m is respectively and independently selected from the arbitrary integer more than or equal to 0.
Preferably, R1And R2It is respectively and independently selected from flowering structure:
R3、R4、R5、R6And R7It is respectively and independently selected from flowering structure:
R8Selected from flowering structure:
N, m is respectively and independently selected from 0,1,2 or 3.
It is highly preferred that more Ammonia dithiocarbonic acid sulfite derivatives shown in formula (1) are selected from following compound:
Compound 1
Compound 2
Compound 3
Compound 4
Compound 5
Compound 6
Compound 7
Compound 8
Compound 9
Compound 10
Compound 11
Compound 12
Compound 13
Compound 14
Compound 15
Compound 16
Compound 17.
Preferably, the modified polyether is selected from number-average molecular weight and divides equally for 2400 methyl butenol polyoxyethylene ether or number
The methylallyl alcohol polyoxyethylene ether that son amount is 2700, the methyl butenol polyoxyethylene ether is by prenol and ethylene oxide
It synthesizes under the action of catalyst, the methylallyl alcohol polyoxyethylene ether is by methylallyl alcohol and ethylene oxide in catalyst action
Lower synthesis.
The present invention also provides the preparation methods of the polycarboxylate water-reducer, the specific steps are as follows:
It weighs each raw material component respectively in proportion, modified polyether, water, acrylic acid and persulfuric acid is successively added into reaction kettle
Ammonium, after completely dissolution, the reproducibility-chain-transferring agent solution for adding 25% are reacted, and are reacted 4-6 hours, are clarified, thoroughly
Bright colourless or weak yellow liquid, adds water to be made into the polycarboxylate water-reducer of different solid contents.
Preferably, the reaction is reacted under -20-50 DEG C of natural room temperature, without heating.
Polycarboxylate water-reducer provided by the invention, due to using reproducibility-chain in the preparation process of the polycarboxylate water-reducer
The more Ammonia dithiocarbonic acid sulfite derivatives of transfer agent replace traditional reductant Vc and chain-transferring agent thioacetic acid or mercapto
Base propionic acid, not only can to avoid due to thioacetic acid or mercaptopropionic acid foul smell, strong corrosive to the toxic action of human body and
Pollution on the environment, and process flow is simplified, it can synthesize at normal temperature, improve serious forgiveness.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
A kind of polycarboxylate water-reducer is specifically prepared by the raw material of following parts by weight through " one kettle way ": modified polyether
Reproducibility-chain-transferring agent solution 12g of 150g, water 150g, acrylic acid 17.5g, ammonium persulfate 1g and 25%；Wherein, above-mentioned
Modified polyether is the methyl butene for being 2400 by the number-average molecular weight that prenol and ethylene oxide synthesize under the action of catalyst
Alcohol polyoxyethylene ether；
Above-mentioned reproducibility-chain-transferring agent is compound 2, and concrete structure formula is as follows,
Compound 2
25% reproducibility-chain-transferring agent the solution is specific the preparation method comprises the following steps: under the conditions of ice-water bath, 500ml's
In reaction flask, 80% hydrazine hydrate 15.6g, 30% dimethylamine agueous solution 75g and 150ml water are sequentially added, in stirring
The lower solution that 15g paraformaldehyde and 200ml water is added dropwise and is formed, time for adding take around 1h, are added dropwise, react 0.5h, remove
Ice-water bath is removed, the reaction was continued 2h forms transparent, clear colourless solution.Sodium hydrogensulfite 104g is continuously added, 3h is reacted, Gu
Body all dissolves, and stops reaction, adds water to be configured to 25% solution, save backup.
The preparation method of the polycarboxylate water-reducer, specific steps are as follows: weigh raw material methyl butenol polyoxyethylene ether respectively
Reproducibility-chain-transferring agent solution 12g of 150g, water 150g, acrylic acid 17.5g, ammonium persulfate 1g and 25%；Successively to poly-
It closes in reaction kettle and above-mentioned base butenol polyoxyethylene ether, water, acrylic acid and ammonium persulfate is added, be stirred and sufficiently dissolve
Afterwards, the reproducibility-chain-transferring agent solution for adding the 25% of above-mentioned preparation, is reacted at 15 DEG C of environment temperature, without adding
Heat, specific reaction 4 hours, is clarified, clear solution, adds water 3.25g to be made into the polycarboxylate water-reducer that solid content is 50% female
Liquid.
Embodiment 2
A kind of slump retaining agent of polycarboxylate water-reducer provided by embodiment 1 specifically passes through " one by the raw material of following parts by weight
Pot method " is prepared: reproducibility-chain of modified polyether 160g, water 300g, acrylic acid 16.9g, ammonium persulfate 1g and 25%
Shift agent solution 12.1g；Wherein, above-mentioned modified polyether is the number synthesized under the action of catalyst by prenol and ethylene oxide
The methyl butenol polyoxyethylene ether that average molecular weight is 2400；Above-mentioned reproducibility-chain-transferring agent is compound 2,25% reduction
Property-specifically the preparation method is the same as that of Example 1 for chain-transferring agent solution.
The preparation method of the slump retaining agent of the polycarboxylic acids, specific steps are as follows: weigh the different methyl butenol polyoxy second of raw material respectively
Reproducibility-chain-transferring agent solution 12.1g of alkene ether 160g, water 300g, acrylic acid 16.9g, ammonium persulfate 1g and 25%；According to
It is secondary that above-mentioned methyl butenol polyoxyethylene ether, water, acrylic acid and ammonium persulfate are added into polymerization reaction kettle, it is stirred and fills
After dividing dissolution, reproducibility-chain-transferring agent solution of the 25% of above-mentioned preparation is added, is reacted at 20 DEG C of environment temperature,
Without heating, specific reaction 4 hours is clarified, clear solution is polycarboxylic acid slump retaining agent mother liquor.
Net slurry experiment: polycarboxylate superplasticizer mother liquor 0.9g, water 87g, the cement 300g that embodiment 1 is provided, it is net in cement
It starches in blender (NJ-160B), stirs 120 seconds slowly, stops 15 seconds, stir fastly 120 seconds, the net slurry flowing of cement is 310mm.
Concrete flowability experiment: cement 260kg, miberal powder 90kg, river sand 200kg, artificial sand 730kg, stone 930kg,
In addition water 165kg configures the polycarboxylate superplasticizer mother liquor 15g of the offer of embodiment 1, the polycarboxylic acid slump retaining agent 3g that embodiment 2 provides
2- is mixed in above-mentioned substance by the solution formed with 66g water in single horizontal shaft forced type concrete mixer (HJW-30 type)
3min, slump 270mm, the slump after one hour is 268mm, almost without loss.
Embodiment 3
A kind of polycarboxylate water-reducer is specifically prepared by the raw material of following parts by weight through " one kettle way ": modified polyether
Reproducibility-chain-transferring agent solution 18.3g of 150g, water 260g, acrylic acid 18.48g, ammonium persulfate 1g and 25%；Wherein,
Above-mentioned modified polyether is the first for being 2700 by the number-average molecular weight that methylallyl alcohol and ethylene oxide synthesize under the action of catalyst
Base propenyl polyoxyethylene ether；Above-mentioned reproducibility-chain-transferring agent is compound 9, and concrete structure formula is as follows,
Compound 9
Above-mentioned reproducibility-chain-transferring agent solution is 25% solution of compound 9, it is specific the preparation method is as follows:
Under the conditions of ice-water bath, in the reaction flask of 500ml, ethylenediamine 15g, 1H-1,2,4- triazoles are sequentially added
34.5g and 150ml water, is added dropwise the solution that 15g paraformaldehyde and 100ml water are formed under stirring, and time for adding about needs
1h is wanted, is added dropwise, 0.5h is reacted, removes ice-water bath, the reaction was continued 2h forms transparent, clear colourless solution.It continuously adds
Carbon disulfide 7.6g is added dropwise in acrylic acid 7.4g, and 1h is dripped off, and reacts 3h, and sodium hydrogensulfite 104g is added, and reacts 3h, and solid is whole
Dissolution stops reaction, adds water to be configured to 25% solution, save backup.
The preparation method of the polycarboxylate water-reducer, specific steps are as follows: weigh raw material methylallyl alcohol polyoxyethylene ether respectively
150g, water 260g, acrylic acid 18.48g, ammonium persulfate 1g and reproducibility-chain-transferring agent solution 18.3g；It is successively anti-to polymerization
It answers and above-mentioned methylallyl alcohol polyoxyethylene ether, water, acrylic acid and ammonium persulfate is added in kettle, be stirred and after completely dissolution,
Reproducibility-chain-transferring agent the solution for adding the 25% of above-mentioned preparation, is reacted at 38 DEG C of environment temperature, without heating,
Specific reaction 5 hours obtains the polycarboxylate superplasticizer mother liquor that solid content is 40%.
Embodiment 4
A kind of slump retaining agent of polycarboxylate water-reducer provided by embodiment 3 specifically passes through " one by the raw material of following parts by weight
Pot method " is prepared: reproducibility-chain of modified polyether 160g, water 300g, acrylic acid 16.9g, ammonium persulfate 1g and 25%
Shift agent solution 18.3g；Wherein, above-mentioned modified polyether is synthesized by methylallyl alcohol with ethylene oxide under the action of catalyst
The methylallyl alcohol polyoxyethylene ether that number-average molecular weight is 2700；Above-mentioned reproducibility-chain-transferring agent be compound 2,25% also
Originality-specific preparation method of chain-transferring agent solution is the same as embodiment 3.
The preparation method of the slump retaining agent of the polycarboxylate water-reducer, specific steps are as follows:
Raw material methylallyl alcohol polyoxyethylene ether 160g, water 300g, acrylic acid 16.9g, ammonium persulfate 1g are weighed respectively, with
And 25% reproducibility-chain-transferring agent solution 18.3g；Above-mentioned methylallyl alcohol polyoxyethylene is successively added into polymerization reaction kettle
Ether, water, acrylic acid and ammonium persulfate, are stirred and after completely dissolution, and the reproducibility-chain for adding the 25% of above-mentioned preparation turns
Move agent solution, reacted at 20 DEG C of environment temperature, without heating, specific reaction 4 hours, clarified, clear solution i.e.
For polycarboxylic acid slump retaining agent mother liquor.
Net slurry experiment: polycarboxylate superplasticizer mother liquor 0.9g, water 87g, the cement 300g that embodiment 3 is provided, it is net in cement
It starches in blender (NJ-160B), stirs 120 seconds slowly, stops 15 seconds, stir fastly 120 seconds, the net slurry flowing of cement is 290mm.
Concrete flowability experiment: cement 260kg, miberal powder 90kg, river sand 200kg, artificial sand 730kg, stone 930kg,
In addition water 165kg configures the polycarboxylate superplasticizer mother liquor 15g of the offer of embodiment 3, the polycarboxylic acid slump retaining agent 3g that embodiment 4 provides
2- is mixed in above-mentioned substance by the solution formed with 66g water in single horizontal shaft forced type concrete mixer (HJW-30 type)
3min, slump 270mm, the slump after one hour is 270mm, is not lost.
Embodiment 5
A kind of polycarboxylate water-reducer is specifically prepared by the raw material of following parts by weight through " one kettle way ": modified polyether
Reproducibility-chain-transferring agent solution 15.2g of 350g, water 400g, acrylic acid 42.93g, ammonium persulfate 2.5g and 25%；Its
In, above-mentioned modified polyether is the first for being 2400 by the number-average molecular weight that prenol and ethylene oxide synthesize under the action of catalyst
Base butenol polyoxyethylene ether；
Above-mentioned reproducibility-chain-transferring agent is compound 16, and concrete structure formula is as follows,
Compound 16
25% reproducibility-chain-transferring agent the solution is specific the preparation method comprises the following steps: under the conditions of ice-water bath, 500ml's
In reaction flask, diethylenetriamine 10.3g, 1H- imidazoles 20.4g and 150ml water is sequentially added, 9g poly is added dropwise under stirring
The solution that formaldehyde and 100ml water are formed, time for adding take around 1h, are added dropwise, and react 0.5h, remove ice-water bath, continue
2h is reacted, transparent, clear colourless solution is formed.Sodium hydrogensulfite 93.6g is continuously added, 3h is reacted, solid all dissolves, stops
It only reacts, adds water to be configured to 25% solution, save backup.
The preparation method of the polycarboxylate water-reducer, specific steps are as follows: weigh raw material methyl butenol polyoxyethylene ether respectively
Reproducibility-chain-transferring agent solution 15.2g of 350g, water 400g, acrylic acid 42.93g, ammonium persulfate 2.5g and 25%；Successively
Above-mentioned methyl butenol polyoxyethylene ether, water, acrylic acid and ammonium persulfate are added into polymerization reaction kettle, is stirred and abundant
After dissolution, reproducibility-chain-transferring agent solution of the 25% of above-mentioned preparation is added, is reacted, is not necessarily at 2 DEG C of environment temperature
Heating, specific reaction 6 hours obtain the polycarboxylate water-reducer that solid content is 50%.
Embodiment 6
A kind of slump retaining agent of polycarboxylate water-reducer provided by embodiment 5 specifically passes through " one by the raw material of following parts by weight
Pot method " is prepared: reproducibility-chain of modified polyether 160g, water 300g, acrylic acid 16.9g, ammonium persulfate 1g and 25%
Shift agent solution 12.1g；Wherein, above-mentioned modified polyether is the number synthesized under the action of catalyst by prenol and ethylene oxide
The methyl butenol polyoxyethylene ether that average molecular weight is 2400；Above-mentioned reproducibility-chain-transferring agent is compound 2,25% reduction
Property-specific preparation method of chain-transferring agent solution is the same as embodiment 5.
The preparation method of the slump retaining agent of the polycarboxylate water-reducer, specific steps are as follows: it is poly- to weigh raw material methyl butenol respectively
Reproducibility-chain-transferring agent solution 5.8g of ethylene oxide ether 160g, water 300g, acrylic acid 16.9g, ammonium persulfate 1g and 25%；
Above-mentioned methyl butenol polyoxyethylene ether, water, acrylic acid and ammonium persulfate are successively added into polymerization reaction kettle, is stirred simultaneously
After completely dissolution, the reproducibility-chain-transferring agent solution for adding above-mentioned 25%, is reacted at 20 DEG C of environment temperature, is not necessarily to
Heating, specific reaction 6 hours, is clarified, clear solution is polycarboxylic acid slump retaining agent mother liquor.
Net slurry experiment: polycarboxylate superplasticizer mother liquor 0.9g, water 87g, the cement 300g that embodiment 5 is provided, it is net in cement
It starches in blender (NJ-160B), stirs 120 seconds slowly, stops 15 seconds, stir fastly 120 seconds, the net slurry flowing of cement is 315mm.
Concrete flowability experiment: cement 260kg, miberal powder 90kg, river sand 200kg, artificial sand 730kg, stone 930kg,
In addition water 165kg configures the polycarboxylate superplasticizer mother liquor 15g of the offer of embodiment 5, the polycarboxylic acid slump retaining agent 3g that embodiment 6 provides
2- is mixed in above-mentioned substance by the solution formed with 66g water in single horizontal shaft forced type concrete mixer (HJW-30 type)
3min, slump 280mm, the slump after one hour is 280mm, is not lost.
With embodiment 1 provide polycarboxylate water-reducer and its room temperature without be added dropwise preparation process for existing heating drip
Processing skill and room temperature are added dropwise technique and compare, and simplify in equipment, in terms of cost of investment, make a concrete analysis of as follows:
By taking 10 tons of double kettles of period production capacity as an example, the polycarboxylic acids synthesis factory that 2000 tons/year of yield is calculated:
Technique: the equipment of needs is added dropwise in heating are as follows: and 2 sets of consersion unit, about 240,000 yuan, 5 tons 1, hydro-thermal boiler, about 200,000
Member, thermodynamic cycle pipeline, about 1.2 ten thousand yuan of pipe-line equipment expense；Other, including case is added dropwise, storage tank, the corollary equipments such as water process are about
60000 yuan, manually installed to take 12 yuan, total expense is about 620,000 yuan；Occupied area about 1000m2。
Technique is added dropwise in room temperature: 2 sets of consersion unit, about 80,000 yuan, other include that case/storage tank/water treatment facilities about 40,000 are added dropwise
Member, manually installed to take 20,000 yuan, total expense only needs 140,000 yuan；Occupied area only needs 300m2。
The technique of embodiment 1: 2 sets of consersion unit, about 40,000 yuan, manually installed to take 0.5 ten thousand yuan, total expense only needs 4.5 ten thousand
Member；Occupied area only needs 80m2。
To sum up, the technique of embodiment 1 is compared with technique is added dropwise in heating, and equipment investment saves 57.5 ten thousand yuan, occupied area section
About 920m2；Compared with technique is added dropwise in room temperature, equipment investment saves 9.5 ten thousand yuan, and occupied area saves 220m2。
Meanwhile the polycarboxylate water-reducer and its room temperature provided with embodiment 1 is for preparation process and existing without being added dropwise
Technique is added dropwise in heating and room temperature is added dropwise technique and compares, and serious forgiveness is high, and the process time is short, makes a concrete analysis of as follows:
Heat dropwise reaction: technics comparing is complicated, dissolves 10min, time for adding 1h, reaction time 4-5h, total time 5-
6h。
Room temperature dropwise reaction: technique simplifies very much, dissolves 10min, and A drop adds 120min, and B drop adds 110min, needs
Control time for adding, total time 4-5h.
The technique of embodiment 1: technique more simplifies, and without the dropwise addition that takes time, control, avoids many rings for being easy error
Section, it is only necessary to which all raw materials are sequentially placed into consersion unit, reaction time 4-6h.
Polycarboxylate water-reducer provided by the invention, is not influenced by temperature during the preparation process, generally all at -20-50 DEG C
It can occur sufficiently to polymerize, even if under the influence of high temperature, without worry raw material self-polymerization.Polycarboxylate water-reducer tool obtained
There are excellent dispersibility and dispersion retentivity, while there is low alkali, low chlorine ion, lower shrinkage, pollution-free, low environmental load and bright
The excellent performances such as aobvious economic benefit.
In addition, in polymerization reaction using after above-mentioned reproducibility-chain-transferring agent, do not need plus link transfer agent thioacetic acid or
Mercaptopropionic acid and reductant Vc, import thioacetic acid price will be about using 8 tons/year or so at 30,000 yuan/ton or so；Reducing agent
Vc price will be about using 8 tons/year or so at 3.1 ten thousand yuan/ton or so；Reproducibility-chain-transferring agent production cost about 0.8 ten thousand
Yuan/ton or so, it will be about using 20 tons/year or so；It amounts to, cost-saved 30,000 yuan/ton * 8 tons/year+3.1 ten thousand yuan/ton * 8
Ton/year -0.8 ten thousand yuan/ton of * 20 tons/year=32.8 ten thousand yuan/year.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, and protection scope is unlimited
In this.Those skilled in the art on the basis of the present invention made by equivalent substitute or transformation, the scope of the invention it
It is interior.
Claims (4)
1. a kind of polycarboxylate water-reducer, which is characterized in that be to be prepared by the raw material of following parts by weight through " one kettle way ": modified
150 parts of polyethers, 150-280 parts of water, 16-20 parts of acrylic acid, 1-5 parts of ammonium persulfate and 25% reproducibility-chain-transferring agent it is molten
5-20 parts of liquid；
Reproducibility-the chain-transferring agent is selected from one or more of following compound；
2. polycarboxylate water-reducer according to claim 1, which is characterized in that the modified polyether is selected from number-average molecular weight
The methylallyl alcohol polyoxyethylene ether that 2400 methyl butenol polyoxyethylene ether or number-average molecular weight is 2700, the methyl fourth
Enol polyoxyethylene ether is synthesized by prenol with ethylene oxide under the action of catalyst, the methylallyl alcohol polyoxyethylene ether
It is synthesized under the action of catalyst by methylallyl alcohol with ethylene oxide.
3. the preparation method of polycarboxylate water-reducer according to claim 1, which is characterized in that specific step is as follows:
It weighs each raw material component respectively in proportion, modified polyether, water, acrylic acid and ammonium persulfate is successively added into reaction kettle,
After completely dissolution, the reproducibility-chain-transferring agent solution for adding 25% is reacted, and is reacted 4-6 hours, is clarified, is transparent
Colourless or weak yellow liquid, add water to be made into the polycarboxylate water-reducer of different solid contents.
4. the preparation method of polycarboxylate water-reducer according to claim 3, which is characterized in that the reaction is at -20-50 DEG C
Natural room temperature under reacted, without heating.
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