CN106279557A - A kind of energy saving and environment friendly polycarboxylate water-reducer and preparation method thereof - Google Patents
A kind of energy saving and environment friendly polycarboxylate water-reducer and preparation method thereof Download PDFInfo
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- CN106279557A CN106279557A CN201510295865.XA CN201510295865A CN106279557A CN 106279557 A CN106279557 A CN 106279557A CN 201510295865 A CN201510295865 A CN 201510295865A CN 106279557 A CN106279557 A CN 106279557A
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Abstract
The invention discloses a kind of energy saving and environment friendly polycarboxylate water-reducer and preparation method thereof, relate to chemical building material field.The present invention is made up of following component and percentage by weight: polyethenoxy ether class polymeric monomer 30～50%, comonomer 2～5%, chain-transferring agent 0.05～0.5%, initiator 0.1～0.8%, surplus is water.The present invention uses the method for radical polymerization, with water as solvent, and need not to heat up without firing equipment, production process, need not to dissolve polymeric monomer, technique is simple, be not required to adopt hot expense, three-waste free discharge, environmental protection；Required water of the present invention is tap water or well water, it is not necessary to deionization produces equipment, saves cost of founding the factory；And the advantage such as volume is few, water-reducing rate is high, function of slump protection is good and adaptability with cement is good that this product has.
Description
Technical field
The present invention relates to chemical building material field, be related specifically to a kind of energy saving and environment friendly polycarboxylic acids and subtract
Water preparation and preparation method thereof.
Background technology
Cement water reducing agent refers in the situation not affecting concrete workability, cement consumption is constant
Under, reduce cement mixing water consumption, to reach to improve the additive of concrete strength.In recent years,
Due to the appearance of poly carboxylic acid series water reducer, expand the range of concrete, according to the mix phase
Between the improvement that keeps of diminishing or the slump, improve the performance of concrete, polycarboxylate water-reducer is comb
Shape structural polymer, is made up of anion (polycarboxylic acids) and side chain (polyoxyethylene ether), its
Dispersibility is mainly due to they adsorptions to cement granules, this due to the sun of polymer
Ion is formed with the cation in the aluminate hydrate of preparation and calcium ion interaction, sun
Ion covers and forms the mineral surface with strong adsorption power, water reducer on the surface of silicate
Absorption mineral surfaces overcome between granule draw with ionization power and cause sterically hindered.
Owing to eliminating a part of wrapped water, the flocculent structure of mineral suspensions reduces, and therefore increases
Add mobility.
The most common production method of water reducer has following characteristics:
1. require certain temperature, such as 60 DEG C of constant temperature or the initial temperature of 40 DEG C, they
Minimum requirements first polyethenoxy ether class polymeric monomer is first melted and just can carry out copolyreaction, this
It is accomplished by substantial amounts of heat energy.
2. polycarboxylic acids synthesis technique uses deionized water.
The modal productive prospecting of two above resulted in production cost high, not environmentally, produce
The situation of complex process.
Summary of the invention
The technical problem to be solved is to provide that a kind of technique is simple, low cost, performance
High, the polycarboxylate water-reducer of environmental protection, another object of the present invention is to provide a kind of poly-carboxylic
The preparation method of acid water reducer, solves the problems referred to above with auxiliary.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of energy-saving ring
Guarantor's type polycarboxylate water-reducer, it is characterised in that: it is made up of following component and percentage by weight: poly-
Oxygen ethylene ethers polymeric monomer 30～50%, comonomer 2～5%, chain-transferring agent 0.05～0.5%,
Initiator 0.1～0.8%, surplus is water.
Further technical scheme is, described polyethenoxy ether class polymeric monomer is 1-propenol-3 polyoxy
One in vinyl Ether, isobutene alcohol polyoxyethylene ether, isopentenol polyoxyethylene ether.
Further technical scheme is, described comonomer be acrylic acid, methacrylic acid,
One or both in 2-(Acryloyloxy)ethanol, hydroxyethyl methylacrylate.
Further technical scheme is, described chain-transferring agent be TGA, mercaptopropionic acid,
One or more in sodium allylsulfonate, methylpropene sodium sulfonate.
Further technical scheme is, described initiator is the mixing of Oxidizing and Reducing Agents
Thing, described oxidant is 1:1～2.5:1 with the weight ratio of reducing agent.
Further technical scheme is, described oxidant is hydrogen peroxide, potassium peroxydisulfate, over cure
One or more in acid ammonium, sodium peroxydisulfate, dibenzoyl peroxide；Described reducing agent is grass
Acid sodium, sodium sulfite, L-AA, sodium thiosulfate neutralize one or more.
Further technical scheme is, described a kind of energy saving and environment friendly polycarboxylate water-reducer
Preparation method, comprises the steps:
(1) by the comonomer of above-mentioned percentage by weight, reducing agent, chain-transferring agent, dissolve
As A liquid in the water of 1-2 times of volume；
(2) oxidant of above-mentioned percentage by weight is dissolved in the water of 4-5 times of volume as
B liquid；
(3) by polyethenoxy ether class polymeric monomer and the 0.5-1 times of body of above-mentioned percentage by weight
Long-pending water joins in four-hole boiling flask and stirs 10 minutes；
(4) by A, B liquid in above-mentioned steps, with peristaltic pump, at the uniform velocity and drip adds to step (3)
Four-hole boiling flask in；
(5) react 0.5-1 hour after step (4) dropping, obtain described water reducer.
Further technical scheme also resides in, and the water used is tap water or well water, and outward appearance is clear
Clear bright, electrical conductivity requires to be not more than 2000us/cm.
Use and have the beneficial effects that produced by technique scheme: the present invention uses radical polymerization
The method closed, with water as solvent, and need not to heat up without firing equipment, production process,
Need not to dissolve polymeric monomer, technique is simple, be not required to adopt hot expense, three-waste free discharge, green ring
Protect；Required water of the present invention is tap water or well water, it is not necessary to deionization produces equipment, saves
Found the factory cost；And this product has, and volume is few, water-reducing rate is high, function of slump protection is good and and cement
The advantage such as adaptability is good.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that
Described embodiment is only a part of embodiment of the present invention rather than whole enforcement
Example.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creativeness
The every other embodiment obtained under work premise, broadly falls into the scope of protection of the invention.
Elaborate a lot of detail in the following description so that fully understanding the present invention, but
It is that the present invention can also use other to be different from alternate manner described here to implement, this area
Technical staff can be similar popularization, the therefore present invention in the case of intension of the present invention
Do not limited by following public specific embodiment.
Embodiment 1
1. methacrylic acid 25.0g, sodium sulfite 0.5g, TGA 0.2g, add water 20g,
Stir, standby as A liquid.
2. hydrogen peroxide 2.0g, add water 25g, stirs, standby as B liquid.
3. in equipped with thermometer, the 500ml four-hole boiling flask of mixing plant, add well water: 200g,
Add HPEG (isobutene alcohol polyoxyethylene ether) polymeric monomer 220g, stir 10 minutes.
4. with peristaltic pump, at the uniform velocity and drip adds A liquid and B liquid, A liquid and B liquid time for adding control
System was at 2 hours.
5., after dropping, continue reaction 30 minutes, react complete, make finished product.
This example well water electrical conductivity 800us/cm, feed initial temperature 15 DEG C, production code member
It is designated as: S-001.
Embodiment 2
1. methacrylic acid 25.0g, sodium sulfite 0.5g, TGA 0.2g, add water 20g,
Stir, standby as A liquid.
2. hydrogen peroxide 2.0g, add water 25g, stirs, standby as B liquid.
3. in equipped with thermometer, the 500ml four-hole boiling flask of mixing plant, add shallow well
Water: 120g, adds HPEG (isobutene alcohol polyoxyethylene ether) polymeric monomer 220g, stirs 10
Minute.
4. with peristaltic pump, at the uniform velocity and drip adds A liquid and B liquid, A liquid and B liquid time for adding control
System was at 2 hours.
5., after dropping, continue reaction 30 minutes, react complete, make finished product.
This example well water electrical conductivity 2200us/cm, feed initial temperature 6 DEG C, production code member
It is designated as: S-002.
Embodiment 3
1. acrylic acid 20.0g, L-AA 0.8g, TGA 0.2g, mercaptopropionic acid 0.5g
Add water 25g, stirs, standby as A liquid.
2. hydrogen peroxide 3.0g, add water 24g, stirs, standby as B liquid.
3. in equipped with thermometer, the 500ml four-hole boiling flask of mixing plant, add well water: 200g,
Add HPEG (isobutene alcohol polyoxyethylene ether) polymeric monomer 230g, stir 10 minutes.
4. with peristaltic pump, at the uniform velocity and drip adds A liquid and B liquid, and A liquid feed time is 3 hours,
B liquid feed time is 2 hours.
5., after dropping, continue reaction 30 minutes, react complete, make finished product.
This example well water electrical conductivity 800us/cm, feed initial temperature 8 DEG C, and production code member is remembered
For: S-003.
Embodiment 4
1. methacrylic acid 25.0g, sodium sulfite 0.5g, TGA 0.2g, add water 20g,
Stir, standby as A liquid.
2. hydrogen peroxide 2.0g, add water 24g, stirs, standby as B liquid.
3. in equipped with thermometer, the 500ml four-hole boiling flask of mixing plant, add well water: 120g,
Add HPEG (isobutene alcohol polyoxyethylene ether) polymeric monomer 220g, stir 10 minutes.
4. with peristaltic pump, at the uniform velocity and drip adds A liquid and B liquid, A liquid and B liquid time for adding control
System was at 2 hours.
5., after dropping, continue reaction 30 minutes, react complete, make finished product.
This example well water electrical conductivity 800us/cm, feed initial temperature 10 DEG C, production code member
It is designated as: S-004.
Embodiment 5
1. acrylic acid 15.0g, L-AA 0.3g, mercaptopropionic acid 0.8g, add water 20g,
Stir, standby as A liquid.
2. sodium peroxydisulfate 1.0g, hydrogen peroxide 0.5g, add water 30g, stirs, as B liquid
Standby.
3. in equipped with thermometer, the 500ml four-hole boiling flask of mixing plant, add well water: 200g,
Addition TPEG (isopentenol polyoxyethylene ether) polymeric monomer 230g, sodium allylsulfonate 2.0g,
Stir 10 minutes.
4. with peristaltic pump, at the uniform velocity and drip adds A liquid and B liquid, A liquid and B liquid time for adding control
System was at 3 hours.
5., after dropping, continue reaction 30 minutes, react complete, make finished product.
This example well water electrical conductivity 800us/cm, feed initial temperature 25 DEG C, production code member
It is designated as: S-005.
Embodiment 6
1. acrylic acid 26.0g, L-AA 0.8g, TGA 0.2g, mercaptopropionic acid 0.5g
Add water 25g, stirs, standby as A liquid.
2. Ammonium persulfate. 3.0g, add water 35g, stirs, standby as B liquid.
3. add from the beginning in equipped with thermometer, the 500ml four-hole boiling flask of mixing plant
Water: 180g, adds HPEG (isobutene alcohol polyoxyethylene ether) polymeric monomer 210g, stirs 10
Minute.
4. with peristaltic pump, at the uniform velocity and drip adds A liquid and B liquid, and A liquid feed time is 3 hours,
B liquid feed time is 2 hours.
5., after dropping, continue reaction 30 minutes, react complete, make finished product.
This example tap water electrical conductivity 200us/cm, feed initial temperature 13 DEG C, and product is compiled
Number it is designated as: S-006.
Implementation result
Below by corresponding experiment, verify the water reducer prepared in above-described embodiment 1～6, right
Answer numbered S-001～006, the performance of water reducer that this programme prepare is expanded on further.
(1) experiment is only starched
Use Beijing Jinyu P.O.42.5 cement, according to " outside GBT 8077-2000 concrete
Add agent homogeneity test method ", detect flowing degree of net paste of cement, W/C=0.29, water reducer is mixed
Amount is the solid volume of folding, the results are shown in Table 1.
Table 1 flowing degree of net paste of cement is tested
(2) intensity experiment
Use Beijing Jinyu P.O.42.5, flyash (II grade), breeze (S95), thin fluvial sand
(moisture content 2%), broken pebble (particle diameter 5-30, continuous grading), by the cooperation in table 2
Ratio, the solid volume of the folding in table 1, join with reference to " GB8076-2008 concrete admixture " standard
Concrete processed, concrete NDT result is with reference to table 3.
Table 2 concrete mix (kg/m3)
| Cement | Flyash | Breeze | Sand | Stone |
| 274 | 60 | 76 | 700 | 1145 |
Table 3 concrete performance
In sum, this handicraft product is equal in terms of water-reducing rate, slump control and gain in strength
Have a clear superiority in, and production technology is simple, with short production cycle, low to water quality requirement, reaction
Condition easily controls, production cost is low, production process environmental protection, is suitable for large-scale production.
Claims (8)
1. an energy saving and environment friendly polycarboxylate water-reducer, it is characterised in that: by following component and
Percentage by weight forms: polyethenoxy ether class polymeric monomer 30～50%, comonomer 2～5%,
Chain-transferring agent 0.05～0.5%, initiator 0.1～0.8%, surplus is water.
The energy saving and environment friendly polycarboxylate water-reducer of one the most according to claim 1, it is special
Levy and be: described polyethenoxy ether class polymeric monomer be allyl alcohol polyethenoxy ether, isobutene alcohol gather
One in oxygen vinyl Ether, isopentenol polyoxyethylene ether.
The energy saving and environment friendly polycarboxylate water-reducer of one the most according to claim 1, it is special
Levy and be: described comonomer is acrylic acid, methacrylic acid, 2-(Acryloyloxy)ethanol, methyl
One or both in 2-(Acryloyloxy)ethanol.
The energy saving and environment friendly polycarboxylate water-reducer of one the most according to claim 1, it is special
Levy and be: described chain-transferring agent is TGA, mercaptopropionic acid, sodium allylsulfonate, methyl
One or more in sodium allylsulfonate.
The energy saving and environment friendly polycarboxylate water-reducer of one the most according to claim 1, it is special
Levy and be: described initiator is the mixture of Oxidizing and Reducing Agents, described oxidant and reduction
The weight ratio of agent is 1:1～2.5:1.
The energy saving and environment friendly polycarboxylate water-reducer of one the most according to claim 1, it is special
Levy and be: described oxidant is hydrogen peroxide, potassium peroxydisulfate, Ammonium persulfate., sodium peroxydisulfate, mistake
One or more in oxidation dibenzoyl；Described reducing agent be Disodium oxalate., sodium sulfite,
L-AA, sodium thiosulfate neutralize one or more.
7. energy saving and environment friendly poly-according to the one described in claim 1-6 any one claim
The preparation method of carboxylic acid water reducer, it is characterised in that: comprise the steps:
(1) by the comonomer of above-mentioned percentage by weight, reducing agent, chain-transferring agent, dissolve
As A liquid in the water of 1-2 times of volume；
(2) oxidant of above-mentioned percentage by weight is dissolved in the water of 4-5 times of volume as
B liquid；
(3) by polyethenoxy ether class polymeric monomer and the 0.5-1 times of body of above-mentioned percentage by weight
Long-pending water joins in four-hole boiling flask and stirs 10 minutes；
(4) by A, B liquid in above-mentioned steps, with peristaltic pump, at the uniform velocity and drip adds to step (3)
Four-hole boiling flask in；
(5) react 0.5-1 hour after step (4) dropping, obtain described water reducer.
8. energy saving and environment friendly poly-according to the one described in claim 1-6 any one claim
Carboxylic acid water reducer, it is characterised in that: the water used is tap water or well water, and outward appearance clarification is thoroughly
Bright, electrical conductivity requires to be not more than 2000us/cm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659175A (en) * | 2017-03-28 | 2018-10-16 | 北新集团建材股份有限公司 | A kind of method preparing polycarboxylate water-reducer and a kind of retarder and preparation method thereof |
| CN109836539A (en) * | 2019-01-28 | 2019-06-04 | 山西科腾环保科技股份有限公司 | A kind of polycarboxylic-acid high water reduction slump retaining agent and preparation method thereof and application method |
| CN111393584A (en) * | 2020-03-26 | 2020-07-10 | 山西佳维新材料股份有限公司 | Polycarboxylate superplasticizer and preparation method and application thereof |
| CN112851879A (en) * | 2021-01-11 | 2021-05-28 | 科之杰新材料集团(贵州)有限公司 | Polycarboxylate superplasticizer for concrete and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775107A (en) * | 2010-02-03 | 2010-07-14 | 北京冶建特种材料有限公司 | Preparation method of concrete polycarboxylate water-reducer at normal temperature |
-
2015
- 2015-06-02 CN CN201510295865.XA patent/CN106279557A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775107A (en) * | 2010-02-03 | 2010-07-14 | 北京冶建特种材料有限公司 | Preparation method of concrete polycarboxylate water-reducer at normal temperature |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659175A (en) * | 2017-03-28 | 2018-10-16 | 北新集团建材股份有限公司 | A kind of method preparing polycarboxylate water-reducer and a kind of retarder and preparation method thereof |
| CN109836539A (en) * | 2019-01-28 | 2019-06-04 | 山西科腾环保科技股份有限公司 | A kind of polycarboxylic-acid high water reduction slump retaining agent and preparation method thereof and application method |
| CN111393584A (en) * | 2020-03-26 | 2020-07-10 | 山西佳维新材料股份有限公司 | Polycarboxylate superplasticizer and preparation method and application thereof |
| CN112851879A (en) * | 2021-01-11 | 2021-05-28 | 科之杰新材料集团(贵州)有限公司 | Polycarboxylate superplasticizer for concrete and preparation method thereof |
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