CN106632742A - Composite activator system and method for preparing concrete water-reducing admixture from same - Google Patents
Composite activator system and method for preparing concrete water-reducing admixture from same Download PDFInfo
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- CN106632742A CN106632742A CN201611262956.4A CN201611262956A CN106632742A CN 106632742 A CN106632742 A CN 106632742A CN 201611262956 A CN201611262956 A CN 201611262956A CN 106632742 A CN106632742 A CN 106632742A
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- water
- exciting agent
- mixed
- activator
- initiator
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Classifications
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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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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
- C04B24/2688—Copolymers containing at least three different monomers
-
- 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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- 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 provides a composite activator system. The system comprises an activator a and an activator b, wherein the activator a is prepared from a peroxide initiator and an azo initiator through mixing, the activator b is prepared from a weak reducing agent and a strong reducing agent through mixing, and the dosage of the activator a is larger than that of the activator b. The composite activator system has the benefits as follows: activation energy needed for reaction is reduced, the reaction time is shortened, and the reaction can be performed at the normal temperature; on the basis of an existing initiator system and a chain transfer agent, the composite activator system is additionally applied, so that conversion rate of the water-reducing admixture can be increased, the use quantity of the raw materials is reduced, and synthesis cost is reduced; besides, water-retention and slump-retaining short-chain branches are introduced to branches, and water-reducing rate and slump-retaining property are improved; performance of inherent auxiliary materials in the initiator system and the chain transfer agent system of a water-reducing admixture synthesis system is not affected by the activators. The invention further discloses a method for preparing a concrete water-reducing admixture. The technological process is concise, and the water-reducing admixture has good property.
Description
Technical field
The present invention relates to cement water reducing agent synthesis technical field, and in particular to a kind of combined type exciting agent system and its use
In the method for preparing cement water reducing agent.
Background technology
With being in full swing for China's basis retrieval, the architectural concrete amount such as railway, highway, bridge increases
Plus.Meanwhile, the production of durable, weather-proof, high-strength contour performance concrete becomes increasingly dependent on high-performance water reducing agent, especially railway
Build, popularized in an all-round way and used high performance water reducing agent of polyocarboxy acid.
In building-up process, the radical polymerization of alkene needs to cause polycarboxylate water-reducer, needs to enter under the high temperature conditions
Row reaction, and course of reaction is exothermic process, the temperature in course of reaction is wayward；Meanwhile, heating needs to consume one surely
Source, high cost；And usually 40% the monomer containing required 340-390 parts (1000 parts of overall reaction liquid meter) admittedly, monomer consumption is big,
High cost.
In sum, be badly in need of a kind of good water-reducing effect, low cost and the water reducer that is readily produced to solve prior art in
The problem of presence.
The content of the invention
Present invention aim at provide one kind and activation energy needed for reaction being greatly reduced, the reaction time can be reduced, guaranteed instead
The combined type exciting agent system of high performance water-reducer cost should be able to be carried out, raw material dosage can be reduced and reduced under normal temperature condition,
Concrete technical scheme is as follows：
A kind of combined type exciting agent system, the system includes exciting agent a and exciting agent b；
The exciting agent a by according to peroxide initiator and azo-initiator according to 1-3：1 quality proportioning mixing
Form；
The exciting agent b is by weak reductant and strong reductant according to 5-10：1 quality proportioning is mixed.
Preferred in above technical scheme, the peroxide initiator is by hydrogen peroxide, ammonium persulfate and benzoyl peroxide
Formyl is according to 6：3-4：1-2 quality proportionings are mixed；The azo-initiator is by azodiisobutyronitrile (AIBN) and azo
Two different heptonitriles are according to 3：The quality proportioning of 0.5-1 is mixed.
Preferred in above technical scheme, the weak reductant is by vitamin C, sodium pyrosulfite, ferrous ion compound
According to 100：10：The quality proportioning of 1-2 is mixed, and the ferrous ion compound is ferrous sulfate, ferrous nitrate, silicic acid Asia
At least one in iron, ferrous hydroxide, sulphur hydrogenation ferrous iron and ferrous bromide；The strong reductant is sodium bisulphite first
Aldehyde.
Using the combined type exciting agent system of the present invention, effect is：(1) activation energy needed for reaction can be greatly reduced, can be with
Reduce the reaction time；(2) using the combination of peroxide initiator and azo-initiator, half-life shorter peroxide draws
Send out agent lay particular emphasis on low temperature can start reaction, can ensure that react carry out under normal temperature condition, without the need for heating energy source, saved into
This；Half-life longer azo-initiator lays particular emphasis on the synthesis of high temperature class, improves conversion ratio, can reduce monomer consumption；(3) match
Vitamin C is used, and the consumption of exciting agent b is slightly above exciting agent a (the i.e. micro- excess of reducing agent), equivalent to a part of chain-transferring agent
Effect, so as to improving Synthesis conversion；The use of organic carbohydrate reducing agent can introduce polyhydroxy group, form hydrogen bond, carry
High-water performance, water keeps, and workability can get well, while protect to collapse also can improve；(4) exciting agent is not single due to being architecture
Single has been catalytic action, and it can also affect the structure of finished product (water reducer) so as to side chain and product (concrete in prior art
Water reducer) it is different, it is more to there is side chain, is favorably improved water-reducing rate, expands its range of application.
Invention additionally discloses a kind of above-mentioned combined type exciting agent system be used for prepare cement water reducing agent method, including with
Lower step：
The first step, addition bed material, specifically：Polymeric monomer, oxidant and water are added into polymer reactor by proportioning；Polymerization
Agitating device in reactor is stirred, and stir speed (S.S.) is 200-1000r/min；
Second step, reaction, specifically：The bed material of dropping liquid A to polymer reactor is initially charged, dropwise addition is added after half an hour
Liquid B, obtains reactant liquor；
The dropping liquid A is by the combination of both exciting agent a and water or by exciting agent a, alkyl acrylate and water three
Combination mix by proportioning；
The dropping liquid B is mixed by acrylic acid, TGA, exciting agent b and water by proportioning；
3rd step, reactant liquor is obtained final product for catalyzing and synthesizing cement water reducing agent through subsequent reactions.
Preferred in above technical scheme, in terms of 1000 parts of overall reaction liquid, the consumption of the polymeric monomer, oxidant and water is
275-340 parts, 1-3 parts and 350-420 parts, the dropping liquid A is by 4-6 part exciting agent a, 0-50 part alkyl acrylates and 80-
120 parts of water are mixed, and the dropping liquid B is by 60-90 part acrylic acid, 1-3 part TGAs, 1-3 part exciting agent b and 50-80
Part water is mixed.
Preferred in above technical scheme, the polymeric monomer is polycarboxylate water-reducer monomer；The oxidant is hydrogen peroxide；
The alkyl acrylate is hydroxy-ethyl acrylate, dodecylacrylate, alkyl methacrylate, octadecyl
At least one in base ester and methyl methacrylate.
Preferred in above technical scheme, the temperature reacted in the second step is normal temperature；During the dropwise addition of the dropping liquid A
Between be 75-90 minutes, the time for adding of the dropping liquid B is 50-60 minutes.
Preferred in above technical scheme, the subsequent reactions in the 3rd step include acid-base neutralization reaction, the soda acid
Neutralization reaction is specifically：Second step gained reactant liquor is neutralized using 30% liquid caustic soda, pH value is adjusted into 5-8.
The combined type exciting agent system of the present invention is used for the method for preparing cement water reducing agent, and effect is：(1) processing step
Simplify, technological parameter is easily controlled；(2) polymeric monomer is a kind of short main chain, the polymeric monomer of long-chain branch, by the covering of long-chain branch and
Adsorption capacity also has space steric effect, reaches a good water-reducing effect (specifically：Gained 35% or so of the invention contains admittedly
Finished product can reach the effect of conventional 40% finished product for containing admittedly)；(3) synthesized by the way of most saving raw material, reduce production
Cost；(4) action principle of water reducer：Water reducer is typically a kind of surfactant, belongs to anionic surfactant；It inhales
Investing cement particle surface makes particle show electrical property, mutually exclusive due to band identical charges between particle, makes cement granules quilt
Disperse and discharge moisture unnecessary between particle and produce water-reduction；On the other hand, after due to adding water reducer, cement granules table
Face forms absorption film, affects the hydration rate of cement, makes the growth of Behavior of Hardened Cement Paste crystal more sophisticated, reduces the capillary of moisture evaporation
Space, network structure is more fine and close, improves the hardness and compact structure of cement mortar；The function of water reducer is：Make cement
Particle disperses, and improves workability, reduces water consumption, so as to improve the compactness and hardness of cement-based material, increases its mobility.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.
Below with reference to specific embodiment, the present invention is further detailed explanation.
Specific embodiment
Technical scheme is described in detail with reference to embodiments, but the present invention can be wanted according to right
The multitude of different ways for limiting and covering is asked to implement.
Embodiment 1：
A kind of preparation method of cement water reducing agent, detailed process is as follows：
Synthetic method specifically includes following steps：
The first step, addition bed material, specifically：300g polymeric monomers, 3g oxidants and 350g water are added into polymer reactor；
Agitating device in polymer reactor is stirred, and stir speed (S.S.) is 350r/min；
Second step, reaction, specifically：The bed material of dropping liquid A to polymer reactor is initially charged, dropping liquid B is added, is obtained
Reactant liquor；
The dropping liquid A is mixed by 10g alkyl acrylates, 6g exciting agent a and 80g water, and the exciting agent a is by mistake
Peroxide initiator and azo-initiator are according to 3：1 quality proportioning is mixed, and the peroxide initiator is by peroxide
Change hydrogen, ammonium persulfate and benzoyl peroxide according to 6：3：1 quality proportioning is mixed, and the azo-initiator is by azo
Bis-isobutyronitrile and ABVN are according to 3：1 quality proportioning is mixed；The alkyl acrylate is acrylic acid hydroxyl second
Ester.
By 3g TGAs, 60g acrylic acid, 3g exciting agent b, (consumption of exciting agent b is less than exciting agent a to the dropping liquid B
Consumption) and 60g water mix, the exciting agent b is by weak reductant and strong reductant according to 5：1 quality proportioning mixing and
Into the weak reductant is by vitamin C, sodium pyrosulfite and ferrous ion compound according to 100：10：1 quality proportioning mixing
Form；The ferrous ion compound is by ferrous sulfate and ferrous nitrate according to 1：1 quality proportioning is mixed；It is described strong also
Former agent is sodium bisulphite formaldehyde.
3rd step, reactant liquor is obtained final product for catalyzing and synthesizing cement water reducing agent through subsequent reactions.
Above-mentioned polymeric monomer is polycarboxylate water-reducer monomer, also has sterically hindered effect by the covering and adsorption capacity of long-chain branch
Should, reach the effect of a diminishing.
The oxidant is hydrogen peroxide.
The sodium bisulphite formaldehyde also known as rongalite, are translucent white oblique square crystal or fritter, its apparent density
1.80-1.85g/cm3, 64 DEG C of its fusing point (is dissolved in its crystallization water), and it is higher than 120 DEG C of decomposition, and its is soluble in water and is slightly soluble in alcohol.
The temperature reacted in above-mentioned second step is normal temperature；The time for adding of the dropping liquid A is 90 minutes, the dropping liquid
The time for adding of B is 60 minutes.
Subsequent reactions in above-mentioned 3rd step include acid-base neutralization reaction, and details are：Using 30% liquid caustic soda to second step
Gained reactant liquor is neutralized, and pH value is adjusted into 6-7.
Embodiment 2
The difference from Example 1 of embodiment 2 is as follows：
In the first step：The consumption of polymeric monomer, oxidant and water is 275g, 1g and 420g；The stirring of agitating device
Speed is 200r/min.
In the second step：The dropping liquid A is mixed by 4g exciting agent a, 15g alkyl acrylates and 120g water,
The exciting agent a is by peroxide initiator and azo-initiator according to 1：1 quality proportioning is mixed, the peroxidating
Thing initiator is by hydrogen peroxide, ammonium persulfate and benzoyl peroxide according to 3：2：1 quality proportioning is mixed, the azo
Class initiator is by azodiisobutyronitrile and ABVN according to 6：1 quality proportioning is mixed；The acrylic acid alkyl
Ester is by hydroxy-ethyl acrylate, dodecylacrylate and methyl methacrylate according to 1：1：1 quality proportioning is mixed.
The dropping liquid B is mixed by 2g TGAs, 90g acrylic acid, 1g exciting agent b and 80g water, the exciting agent
B is by weak reductant and strong reductant according to 10：1 quality proportioning is mixed；The weak reductant is by vitamin C, burnt sulfurous
Sour sodium and ferrous ion compound are according to 50：5：1 quality proportioning is mixed；The ferrous ion compound is that sulfuric acid is sub-
Iron.
Other processing steps, technological parameter etc. are same as Example 1.
Embodiment 3
The difference from Example 1 of embodiment 3 is as follows：
In the first step：The consumption of polymeric monomer, oxidant and water is 340g, 2g and 400g；The stirring of agitating device
Speed is 1000r/min.
In the second step：The dropping liquid A is mixed by 5g exciting agent a, 50g alkyl acrylates and 100g water,
The exciting agent a is by peroxide initiator and azo-initiator according to 2：1 quality proportioning is mixed, the peroxidating
Thing initiator is by hydrogen peroxide, ammonium persulfate and benzoyl peroxide according to 6：4：1 quality proportioning is mixed, the azo
Class initiator is by azodiisobutyronitrile and ABVN according to 3：0.8 quality proportioning is mixed；The alkyl acrylate
Base ester is hydroxy-ethyl acrylate, dodecylacrylate, alkyl methacrylate, octadecyl acrylate and methyl-prop
E pioic acid methyl ester installs 1：2：2：1：3 quality proportioning is mixed.
The dropping liquid B is mixed by 80g acrylic acid, 2g exciting agent b, 1g TGAs and 70g water, the exciting agent
B is by weak reductant and strong reductant according to 8：1 quality proportioning is mixed；The weak reductant is by vitamin C, pyrosulfurous acid
Sodium and ferrous ion compound are according to 200：20：3 quality proportioning is mixed；The ferrous ion compound is sub- by sulfuric acid
Iron, ferrous hydroxide, sulphur hydrogenation ferrous iron and ferrous bromide are according to 1：1：1：1 quality proportioning is mixed.
Other processing steps, technological parameter etc. are same as Example 1.
The gained cement water reducing agent of above-described embodiment 1- embodiments 3 and ordinary water-reducing agent are tested respectively, mother liquor is dense on an equal basis
Cement paste initial fluidity under degree and mobility during Jing, refer to table 1.Experiment cement used is new 42.5 ordinary portland cement of China,
With reference to GB/8076-2008《Concrete admixture》Testing standard.
The different Water-reducing Admixtures To Cements of table 1 starch flow effect only
| Water reducer species | Initial fluidity/mm | Mobility/mm during Jing |
| Ordinary water-reducing agent | 250 | 220 |
| Embodiment 1 | 261 | 265 |
| Embodiment 2 | 263 | 260 |
| Embodiment 3 | 262 | 272 |
It can be seen from table 1：The initial fluidity of embodiment of the present invention 1-3 is big compared with ordinary water-reducing agent mother liquor, and during Jing
Mobility compared with initial fluidity more preferably, therefore, the Chain System of method of the present invention gained cement water reducing agent is more reasonable, has
Beneficial to raising dispersion stabilization, it is ensured that function of slump protection is significantly improved.
The preferred embodiments of the present invention are the foregoing is only, the present invention is not limited to, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (8)
1. a kind of combined type exciting agent system, it is characterised in that the system includes exciting agent a and exciting agent b；
The exciting agent a is by peroxide initiator and azo-initiator according to 1-3：1 quality proportioning is mixed；
The exciting agent b is by weak reductant and strong reductant according to 5-10：1 quality proportioning is mixed.
2. combined type exciting agent system according to claim 1, it is characterised in that the peroxide initiator is by peroxide
Change hydrogen, ammonium persulfate and benzoyl peroxide according to 6：3-4：The quality proportioning of 1-2 is mixed；
The azo-initiator is by azodiisobutyronitrile and ABVN according to 3：0.5-1 quality proportioning mixing and
Into.
3. combined type exciting agent system according to claim 1, it is characterised in that the weak reductant is by vitamin C, Jiao
Sodium sulfite and ferrous ion compound are according to 100：10：The quality proportioning of 1-2 is mixed, and the ferrous ion compound is
At least one in ferrous sulfate, ferrous nitrate, ferrous metasilicate, ferrous hydroxide, sulphur hydrogenation ferrous iron and ferrous bromide；
The strong reductant is sodium bisulphite formaldehyde.
4. a kind of combined type exciting agent system as described in claim 1-3 any one is used to prepare the side of cement water reducing agent
Method, it is characterised in that comprise the following steps：
The first step, addition bed material, specifically：Polymeric monomer, oxidant and water are added into polymer reactor by proportioning；Polymerisation
Agitating device in device is stirred, and stir speed (S.S.) is 200-1000r/min；
Second step, reaction, specifically：The bed material of dropping liquid A to polymer reactor is initially charged, dropping liquid B is added after half an hour,
Obtain reactant liquor；
Combinations or knot by exciting agent a, alkyl acrylate and water three of the dropping liquid A by both exciting agent a and water
Conjunction is mixed by proportioning；
The dropping liquid B is mixed by acrylic acid, TGA, exciting agent b and water by proportioning；
3rd step, reactant liquor is obtained final product into cement water reducing agent through subsequent reactions.
5. the method for preparing cement water reducing agent according to claim 4, it is characterised in that with 1000 parts of overall reaction liquid
Meter, the consumption of the polymeric monomer, oxidant and water is 275-340 parts, 1-3 parts and 350-420 parts, and the dropping liquid A is by 4-6 parts
Exciting agent a, 0-50 part alkyl acrylate and 80-120 part water are mixed, and the dropping liquid B is by 60-90 part acrylic acid, 1-3
Part TGA, 1-3 part exciting agent b and 50-80 part water are mixed.
6. the method for preparing cement water reducing agent according to claim 5, it is characterised in that the polymeric monomer is polycarboxylic acids
Water reducer monomer；The oxidant is hydrogen peroxide；The alkyl acrylate is hydroxy-ethyl acrylate, lauryl base
At least one in ester, alkyl methacrylate, octadecyl acrylate and methyl methacrylate.
7. the method for preparing cement water reducing agent according to claim 4, it is characterised in that react in the second step
Temperature is normal temperature；The time for adding of the dropping liquid A is 75-90 minutes, and the time for adding of the dropping liquid B is 50-60 minutes.
8. the method for preparing cement water reducing agent according to claim 4, it is characterised in that follow-up in the 3rd step
Reaction includes acid-base neutralization reaction, and the acid-base neutralization reaction is specifically：Liquid caustic soda using 30% is anti-by second step gained
Answer liquid to be neutralized, pH value is adjusted into 5-8.
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| CN201611262956.4A CN106632742A (en) | 2016-12-30 | 2016-12-30 | Composite activator system and method for preparing concrete water-reducing admixture from same |
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| CN201611262956.4A CN106632742A (en) | 2016-12-30 | 2016-12-30 | Composite activator system and method for preparing concrete water-reducing admixture from same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017764A (en) * | 2018-01-19 | 2018-05-11 | 广东乐尔康生物科技股份有限公司 | The method that accessory substance in being produced using ursin prepares polycarboxylic acids mother liquor |
| CN109694510A (en) * | 2018-12-29 | 2019-04-30 | 四川君尚亚克力制造有限公司 | A kind of environmental protection runway pavement material and construction method |
| CN110128603A (en) * | 2019-06-11 | 2019-08-16 | 云南建投高分子材料有限公司 | Stablize the method for synthesis polycarboxylate water-reducer under cryogenic conditions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965415A (en) * | 2014-04-15 | 2014-08-06 | 中国矿业大学(北京) | Method for preparing polycarboxylic acid grafted copolymer superplasticizer |
| CN104448156A (en) * | 2014-11-22 | 2015-03-25 | 萧县鑫固混凝土外加剂有限公司 | Room-temperature preparation method for high-efficiency polycarboxylic acid water reducing agent |
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- 2016-12-30 CN CN201611262956.4A patent/CN106632742A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965415A (en) * | 2014-04-15 | 2014-08-06 | 中国矿业大学(北京) | Method for preparing polycarboxylic acid grafted copolymer superplasticizer |
| CN104448156A (en) * | 2014-11-22 | 2015-03-25 | 萧县鑫固混凝土外加剂有限公司 | Room-temperature preparation method for high-efficiency polycarboxylic acid water reducing agent |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017764A (en) * | 2018-01-19 | 2018-05-11 | 广东乐尔康生物科技股份有限公司 | The method that accessory substance in being produced using ursin prepares polycarboxylic acids mother liquor |
| CN109694510A (en) * | 2018-12-29 | 2019-04-30 | 四川君尚亚克力制造有限公司 | A kind of environmental protection runway pavement material and construction method |
| CN109694510B (en) * | 2018-12-29 | 2021-03-23 | 四川君尚亚克力制造有限公司 | Environment-friendly runway pavement material and construction method |
| CN110128603A (en) * | 2019-06-11 | 2019-08-16 | 云南建投高分子材料有限公司 | Stablize the method for synthesis polycarboxylate water-reducer under cryogenic conditions |
| CN110128603B (en) * | 2019-06-11 | 2021-10-01 | 云南建投高分子材料有限公司 | Method for stably synthesizing polycarboxylate superplasticizer under low-temperature condition |
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Application publication date: 20170510 |