CN104530323B - A kind of preparation method of concrete high-efficiency polycarboxylate water-reducer - Google Patents
A kind of preparation method of concrete high-efficiency polycarboxylate water-reducer Download PDFInfo
- Publication number
- CN104530323B CN104530323B CN201410737268.3A CN201410737268A CN104530323B CN 104530323 B CN104530323 B CN 104530323B CN 201410737268 A CN201410737268 A CN 201410737268A CN 104530323 B CN104530323 B CN 104530323B
- Authority
- CN
- China
- Prior art keywords
- grams
- water
- pipeline
- tank
- reducer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of preparation method of concrete high-efficiency polycarboxylate water-reducer, high-quality water reducer is produced.The step of the method, includes：To be well mixed in the mixture of unsaturated carboxylic acid and its derivative, surfactant and water premix groove A, peroxide and water separately are put into premix groove B is well mixed；The two kinds of liquid that will be premixed in groove A and premix groove B are input in pipeline reactor, the mixed liquor heating that will enter；Mixed liquor carries out polymerisation in pipeline reactor；After completing polymerisation, polymer is obtained, polymer is cooled down, then the acid-base value of polymer is adjusted to neutrality, through drying with salt, obtain high-efficiency polycarboxylic acid water reducer powder.Obtained high-efficiency polycarboxylic acid water reducer steady quality reliability of the invention, simple production process direct motion.
Description
Technical field
The present invention relates to the preparation method of cement water reducing agent, particularly a kind of system of concrete high-efficiency polycarboxylate water-reducer
Preparation Method.
Background technology
Water reducer is a kind of important concrete admixture, is the essential part of cement concrete, and it accounts for outer
Plus more than the 80% of agent total amount.The major function of water reducer is, in the case where keeping the concrete mix slump constant, to subtract
The water consumption of few mixture, improves the rheological property of mixture and improves intensity and anti-freezing property of concrete etc..Water reducer
Development course can be divided into：The first generation with calcium lignosulfonate as representative is plain edition water reducer；The second generation with naphthalene system as representative is efficient
Water reducer；The third generation with polycarboxylic-acid as representative is high-performance water reducing agent.Polycarboxylate water-reducer is a kind of new concrete
Super plasticizer, compared with traditional naphthalene water reducer, there is low-dosage, diminishing high, high-thin arch dam, enhancing high and cement to adapt to for it
Property strong, production and using it is pollution-free the advantages of, in the whole world, many countries have been used widely.Current polycarboxylic acid diminishing
Agent mainly has polyesters water reducer, three kinds of water reducers of common polyether class and high-performance polyethers water reducer.Poly carboxylic acid series water reducer
It is a class ionic graft copolymer, molecular structure is in comb shape, and the free degree is big, and molecular size range is adjustable, can carry out molecule to it
Structure design.Main chain is that, containing carboxyl or sulfonic alkyl carbon chain, side chain is the polyoxyethylene construction unit of different length.Often
The synthetic method of poly carboxylic acid series water reducer is mainly activated monomer copolymerization method, typically with surface-active macromonomer and unsaturated carboxylic
Acid is carried out in copolyreaction, but synthesis technique in aqueous, and temperature and material addition speed have very big to polymerisation
Influence, particularly in production is amplified, due to the defect of traditional reactor so that temperature is difficult precise control, material is added
Local concentration can be caused uneven, and cause that polymerisation degree is uneven, cause polymer molecular weight wider distribution, product
Quality is unstable, and properties of product are low.
The content of the invention
The invention provides a kind of preparation method of concrete high-efficiency polycarboxylate water-reducer, high-quality water reducer is produced.
A kind of preparation method of concrete high-efficiency polycarboxylate water-reducer that the present invention is provided is comprised the following steps：
A. the mixture of unsaturated carboxylic acid and its derivative, surfactant and water in mass ratio 100: 10: 100 is put into
It is well mixed in premix groove A, peroxide and water in mass ratio 1: 4 separately is put into premix groove B is well mixed；
B. the two kinds of liquid that will be premixed in groove A and premix groove B are mixed while entering a pipeline, preliminary in two kinds of liquid
Mix stages are mixed with ultrasonic assistant, it is sufficiently mixed uniformly, obtain mixed liquor, and mixed liquor then is input into duct type
In reactor, the mixed liquor of entrance is heated to 80 DEG C -82 DEG C；
C. mixed liquor flows in pipeline reactor, and carries out polymerisation, and control mixed liquor is in pipeline reactor
Interior flowing velocity, less than or equal to duct length divided by the reaction time, the reaction time is 4 hours to its flowing velocity；
D. mixed liquor obtains polymer after the rear of pipeline reactor completes polymerisation, and polymer is cooled to
30 DEG C -35 DEG C, then the acid-base value of polymer is adjusted to neutrality, neutral polymer liquid is carried out into centrifugal spray drying, add
The inorganic salts of the 50% of polymer quality, are well mixed, that is, obtain high-efficiency polycarboxylic acid water reducer powder.
Unsaturated carboxylic acid and its derivative in the step a are polyoxyethylene methyl acrylate, methacrylic acid,
ALS, polyethylene glycol monomethyl ether, acrylic acid and mercaptopropionic acid；Surfactant is cetyl trimethylammonium bromide
Or ten youngster's sodium alkyl benzene sulfonates；Polymerization catalyst is ammonium persulfate；Acid-base value adjustment in the step b uses NaOH；
Inorganic salts in the step d are calcium carbonate or talcum powder.
It is of the invention compared with existing similar technique, it significantly has the beneficial effect that：
Traditional reactor is become duct type design by the present invention, solves radiating problem, being capable of precise control reaction temperature
Degree, makes each several part thermally equivalent in reaction, reaches accurately reaction temperature, while can the precise control reaction time.By meter
The use of pump is measured, material is uniformly added into, each several part concentration is homogeneous in reaction, particularly the concentration of initiator is equal in reaction solution
Even distribution, constant concentration thus occurs polymerisation stabilization, the product homogeneous so as to obtain quality, polymerizate molecule
Amount narrow distribution, making the high-efficiency polycarboxylic acid water reducer of present invention preparation has good performance, and steady quality reliability.Simultaneously
In order to overcome defect of the pipeline reactor without stirring, agitating function is substituted using ultrasonic wave, reaction mass is sufficiently mixed
It is even, obtain high-quality polymerizate.
Concrete high-efficiency polycarboxylate water-reducer prepared by the present invention, is detected, function admirable using national standard method.Cement
Paste flowing degree method of testing is with reference to GB 8077-2000《Methods for testing uniformity of concrete admixture》Carry out.Concrete diminishing
Rate and compressive strength test are with reference to GB8076-2008《Concrete admixture》Carry out.
Brief description of the drawings
Fig. 1 is a kind of process flow diagram of the preparation method of concrete high-efficiency polycarboxylate water-reducer.
Specific embodiment
The present invention is described in further details with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
As shown in figure 1,800 grams of polyoxyethylene methyl acrylate is added in premixing tank A, 200 grams of methacrylic acid,
200 grams of ALS, 1200 grams of water, 120 grams of cetyl trimethylammonium bromide is stirred and evenly mixed, and uses measuring pump input pipe
In road, 360 milliliters per hour of flow velocity；50 grams of ammonium persulfate is added in premixing tank B, 200 grams of stirring and dissolvings of water are defeated with measuring pump
In entering pipeline, 40 milliliters per hour of flow velocity.Two premixing tank liquid are input into a pipeline and are mixed simultaneously, are tentatively mixed in two liquid
The conjunction stage is radiated with 100W industrial ultrasonics ripple to pipe ultrasonic, and auxiliary makes it be sufficiently mixed uniformly.Well mixed liquid is defeated
Enter pipeline reactor, pipeline reactor is located in heating tank, regulation heating tank temperature makes the pipeline in heating tank to 80 DEG C
80 DEG C are reached, reaction solution flowing reactive in pipeline, the reaction time is 4 hours, obtains polymer.Polymer is entered by pipeline
Cooling bath, cooling bath temperature is 30 DEG C.Polymer after cooling enters neutralizing tank, and neutrality is adjusted to NaOH, obtains bright orange
Color solution, takes 1000 grams of the solution, and centrifugal spray drying adds 50 grams of 1250 mesh calcium carbonate, that is, obtains High-efficiency polycarboxylic acid diminishing
Agent powder.
Performance detection：When water reducer addition is the 0.3% of cement, detection flowing degree of net paste of cement is 260mm.Gassiness
Amount, 3.2%.When initial, slump 19cm, diffusance 48*48cm, after half an hour, slump 20.5cm, diffusance 49*54cm.
Embodiment 2
As shown in figure 1, adding 800 grams of polyethylene glycol monomethyl ether, 200 grams of acrylic acid, mercaptopropionic acid 200 in premixing tank A
Gram, 1200 grams of water, ten 120 grams of youngster's sodium alkyl benzene sulfonates are stirred and evenly mixed, with measuring pump input channel, flow velocity 360 milli per hour
Rise；50 grams of ammonium persulfate of addition, 200 grams of stirring and dissolvings of water in premixing tank B, with measuring pump input channel, flow velocity is per hour
40 milliliters.Two premixing tank liquid are input into a pipeline and are mixed simultaneously, super with 100W industry in two liquid preparatory mix stages
Sound wave is radiated to pipe ultrasonic, and auxiliary makes it be sufficiently mixed uniformly.By in well mixed liquid input tube road formula reactor, manage
Road formula reactor is located in heating tank, and regulation heating tank temperature makes the pipeline in heating tank reach 80 DEG C to 80 DEG C, and reaction solution exists
Flowing reactive in pipeline, the reaction time is 4 hours, obtains polymer.Polymer enters cooling bath, cooling bath temperature by pipeline
It is 30 DEG C.Reaction solution enters neutralizing tank after cooling, and neutrality is adjusted to NaOH, obtains bright yellow solution, takes the solution 1000
Gram, centrifugal spray drying adds 50 grams of 1250 mesh talcum powder, that is, obtain high-efficiency polycarboxylic acid water reducer powder.
Performance detection：When water reducer addition is the 0.3% of cement, detection flowing degree of net paste of cement is 255mm.Gassiness
Amount, 3.0%.When initial, slump 20cm, diffusance 50*52cm, after half an hour, slump 21cm, diffusance 53*52cm.
Claims (2)
1. a kind of preparation method of concrete high-efficiency polycarboxylate water-reducer, it is characterised in that the method is comprised the following steps：Pre-
800 grams of polyoxyethylene methyl acrylate, 200 grams of methacrylic acid, 200 grams of ALS, water are added in mixed tank A
1200 grams, 120 grams of cetyl trimethylammonium bromide is stirred and evenly mixed, with measuring pump input channel, flow velocity 360 milli per hour
Rise；50 grams of ammonium persulfate of addition, 200 grams of stirring and dissolvings of water in premixing tank B, with measuring pump input channel, flow velocity is per hour
40 milliliters；Two premixing tank liquid are input into a pipeline and are mixed simultaneously, super with 100W industry in two liquid preparatory mix stages
Sound wave is radiated to pipe ultrasonic, and auxiliary makes it be sufficiently mixed uniformly；By well mixed liquid input tube road formula reactor, pipeline
Formula reactor is located in heating tank, and regulation heating tank temperature makes the pipeline in heating tank reach 80 DEG C to 80 DEG C, and reaction solution is in pipe
Flowing reactive in road, the reaction time is 4 hours, obtains polymer；Polymer enters cooling bath by pipeline, and cooling bath temperature is
30℃；Polymer after cooling enters neutralizing tank, and neutrality is adjusted to NaOH, obtains bright yellow solution, takes the solution 1000
Gram, centrifugal spray drying adds 50 grams of 1250 mesh calcium carbonate, that is, obtain high-efficiency polycarboxylic acid water reducer powder.
2. a kind of preparation method of concrete high-efficiency polycarboxylate water-reducer, it is characterised in that the method is comprised the following steps：Pre-
800 grams of polyethylene glycol monomethyl ether, 200 grams of acrylic acid, 200 grams of mercaptopropionic acid, 1200 grams of water, detergent alkylate are added in mixed tank A
120 grams of sodium sulfonate, stirs and evenly mixs, with measuring pump input channel, 360 milliliters per hour of flow velocity；Over cure is added in premixing tank B
50 grams of sour ammonium, 200 grams of stirring and dissolvings of water, with measuring pump input channel, 40 milliliters per hour of flow velocity.Two premixing tank liquid are simultaneously
A piece pipeline of input is mixed, and pipe ultrasonic is radiated with 100W industrial ultrasonics ripple in two liquid preparatory mix stages, auxiliary
It is set to be sufficiently mixed uniformly；By in well mixed liquid input tube road formula reactor, pipeline reactor is located in heating tank,
Regulation heating tank temperature makes the pipeline in heating tank reach 80 DEG C, reaction solution flowing reactive in pipeline, reaction time to 80 DEG C
It is 4 hours, obtains polymer；Polymer enters cooling bath by pipeline, and cooling bath temperature is 30 DEG C；Reaction solution enters after cooling
Neutralizing tank, neutrality is adjusted to NaOH, obtains bright yellow solution, takes 1000 grams of the solution, and centrifugal spray drying adds 1250
50 grams of mesh talcum powder, that is, obtain high-efficiency polycarboxylic acid water reducer powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410737268.3A CN104530323B (en) | 2014-12-08 | 2014-12-08 | A kind of preparation method of concrete high-efficiency polycarboxylate water-reducer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410737268.3A CN104530323B (en) | 2014-12-08 | 2014-12-08 | A kind of preparation method of concrete high-efficiency polycarboxylate water-reducer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104530323A CN104530323A (en) | 2015-04-22 |
| CN104530323B true CN104530323B (en) | 2017-05-31 |
Family
ID=52845977
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410737268.3A Active CN104530323B (en) | 2014-12-08 | 2014-12-08 | A kind of preparation method of concrete high-efficiency polycarboxylate water-reducer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104530323B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457578A (en) * | 2015-10-15 | 2016-04-06 | 上海杰深建材有限公司 | Novel liquid water reducer dehydration technology |
| CN113332913A (en) * | 2021-08-04 | 2021-09-03 | 湖南凝英新材料科技有限公司 | Premixing device, production system and production method for polycarboxylate superplasticizer |
| CN113866049A (en) * | 2021-09-27 | 2021-12-31 | 筑友智造建设科技集团有限公司 | 3D printing concrete material pumping control system |
| CN114870785A (en) * | 2021-12-17 | 2022-08-09 | 广东科隆智谷新材料股份有限公司 | Continuous reaction equipment for preparing polycarboxylate superplasticizer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942659A (en) * | 2012-11-16 | 2013-02-27 | 上海台界化工有限公司 | Method for producing polycarboxylic water reducer by tubular reactor |
| CN103537241A (en) * | 2013-10-16 | 2014-01-29 | 北京新奥混凝土集团有限公司 | Single-channel tubular reaction device for producing polycarboxylate superplasticizer |
| CN103980435A (en) * | 2014-05-22 | 2014-08-13 | 武汉华轩高新技术有限公司 | Functionalized regulating and controlling system for production of polycarboxylate water reducer |
-
2014
- 2014-12-08 CN CN201410737268.3A patent/CN104530323B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942659A (en) * | 2012-11-16 | 2013-02-27 | 上海台界化工有限公司 | Method for producing polycarboxylic water reducer by tubular reactor |
| CN103537241A (en) * | 2013-10-16 | 2014-01-29 | 北京新奥混凝土集团有限公司 | Single-channel tubular reaction device for producing polycarboxylate superplasticizer |
| CN103980435A (en) * | 2014-05-22 | 2014-08-13 | 武汉华轩高新技术有限公司 | Functionalized regulating and controlling system for production of polycarboxylate water reducer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104530323A (en) | 2015-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104692700B (en) | Xu puts collapse protective poly-carboxylic acid high-performance water reducing agent and preparation method thereof | |
| CN103553413B (en) | A kind of sticky type polycarboxylate water-reducer and preparation method thereof of adjusting | |
| CN104356300B (en) | Efficient retardation water reducing agent of a kind of modification of chitosan and preparation method thereof and using method | |
| CN104530323B (en) | A kind of preparation method of concrete high-efficiency polycarboxylate water-reducer | |
| CN103772624B (en) | A kind of early-strength type polycarboxylate concrete dehydragent and preparation method thereof | |
| CN104230203A (en) | Super controlled release type polycarboxylate slump retention agent and preparation method thereof | |
| CN106279561B (en) | A kind of viscosity reduction type poly carboxylic acid series water reducer for high performance concrete | |
| CN104098286B (en) | Special concrete pumping agent for ultra-high buildings and preparation method thereof | |
| CN106146749A (en) | Meet polycarboxylate water-reducer of 620 meters of super high pump-conveying self-compacting concretes requirements and preparation method thereof | |
| CN108794700A (en) | A kind of carboxylic acid group polymer and preparation method thereof and sustained-release polycarboxylic water reducer | |
| CN105968239B (en) | The method that electrochemical polymerization prepares polyacrylate | |
| CN104692701B (en) | A kind of normal temperature synthesis type polycarboxylate high performance water-reducing agent and preparation method | |
| CN106279565A (en) | A kind of two excitation system produces solid polycarboxylic acid water reducing agent and preparation method thereof | |
| CN108034024A (en) | A kind of preparation method of high-slump-retentionpolycarboxylate polycarboxylate water reducer | |
| CN105776933A (en) | Mud-resisting type polycarboxylate-type water reducer and preparation method and use method thereof | |
| CN104292396A (en) | Preparation method of dual-control polycarboxylic acid slump retaining agent | |
| CN104725574A (en) | Method for synthesizing solid polyacrylic-series water reducing agents by aid of microwaves at one step | |
| CN106188456A (en) | A kind of preparation method of the modified naphthalene series water-reducing agent being applicable to mud-containing aggregates | |
| CN105461866A (en) | Viscosity-reducing type polycarboxylic-acid water-reducing agent and preparation method thereof | |
| CN104371074A (en) | Low-temperature high-concentration polycarboxylic acid water reducing agent and preparation method thereof | |
| CN208494068U (en) | A kind of polycarboxylic acids water reducing agent compositional apparatus | |
| CN106519137A (en) | Cross-star-shaped slow-release slump-retaining type polycarboxylic-acid water-reducing agent and preparation method thereof | |
| CN106317343A (en) | Water-reducing agent for polycarboxylate concrete and preparation and application thereof | |
| CN102807653A (en) | Co-polycarboxylic acid high efficiency water reducer capable of compounding with naphthalene formaldehyde water reducer and method for preparing same | |
| CN107722189B (en) | A kind of preparation method of rigidity sealing end resistance mud polycarboxylate water-reducer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191024 Address after: 114044 Anshan province hi tech Zone, thousands of mountain road, No. 185, No. Co-patentee after: Bi Wanli Patentee after: University of Science and Technology Liaoning Science Park Development Co., Ltd. Address before: 114044 Anshan province hi tech Zone, thousands of mountain road, No. 185, No. Patentee before: Liaoning Science and Technology Univ. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200525 Address after: 114044 No. 185 Qianshan Middle Road, hi tech Zone, Liaoning, Anshan Patentee after: LIAONING KEDA ZHONGCHI MAGNESIUM BUILDING MATERIAL TECHNOLOGY Co.,Ltd. Address before: 114044 Anshan province hi tech Zone, thousands of mountain road, No. 185, No. Co-patentee before: Bi Wanli Patentee before: Liaoning University of science and Technology Science Park Development Co., Ltd |