CN106397687A - High-adaptability polycarboxylate superplasticizer master batch prepared from all-solid clean raw materials - Google Patents
High-adaptability polycarboxylate superplasticizer master batch prepared from all-solid clean raw materials Download PDFInfo
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- CN106397687A CN106397687A CN201610955668.0A CN201610955668A CN106397687A CN 106397687 A CN106397687 A CN 106397687A CN 201610955668 A CN201610955668 A CN 201610955668A CN 106397687 A CN106397687 A CN 106397687A
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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
- 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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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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
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- Materials Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a high-adaptability polycarboxylate superplasticizer master batch prepared from all-solid clean raw materials. The master batch is applicable to enterprises with high environmental-protection production requirement and poor storage measure safety. With 40% in percentage by mass of a mother solution serving as the limit and the total mass of the synthesis raw materials being 1000, the master batch is prepared from the raw materials in parts by mass as follows: 350-360 parts of polyether macromonomers, 13.2-22.2 parts of small monomers of unsaturated polycarboxylic acids, 7.0-15.0 parts of small monomers of unsaturated anhydrides, 2.0-5.0 parts of a solid oxidant, 0.6-5.0 parts of a solid reductant, 3.0-5.0 parts of a solid chain transfer agent and the balance of water. The synthesized polycarboxylate superplasticizer has moderate molecular weight, multiple carboxyl groups are distributed in a three-dimensional manner, and the adsorption capacity is high; the dosage of polyether is high, the density of branched chains is large, the small monomers of unsaturated anhydrides are hydrolyzed continuously to release carboxyl groups, and the slump retaining capacity is high.
Description
Technical field
The present invention relates to a kind of cement-based gelling material polycarboxylate water-reducer, it is adapted to additive raw material storing, leads to
The not good manufacturing enterprise of wind energy power is and in particular to a kind of high-adaptability polycarboxylate water-reducer of total solids spatter property raw material preparation is female
Material.
Background technology
Concrete admixture production accident generally relates to raw material and technique two aspect, the thing wherein causing with raw material
Therefore it is most commonly seen.The additive industrial chemicals that are related to of production, generally have severe corrosive, also inflammable and explosive, production operation or storage
Deposit not at that time, initiation fire can even explode, cause casualties and device damage.Additive manufacturing enterprise is as far as possible using clear
Clean raw material, the energy, modified technique technology and equipment, accelerate energy-conserving and emission-cutting technology research and development, Promoting Enterprise clean manufacturing, and then promote
The overall development of additive.
In poly carboxylic acid series water reducer with cement granules interaction, the carboxylate radical in conventional raw material propylene acid acts primarily as
Anchorage effect, i.e. adsorption, absorption is the scattered basis of water reducer.Binary acid-itaconic acid, fumaric acid and ternary acid-Aconitum carmichjaelii Debx.
Acid, has more preferable anchoring adsorption compared with acrylic acid, in view of the corresponding matter of unit moles of carboxylic acids root of itaconic acid and equisetic acid
Amount is less, that is, on an equal basis under anchoring absorbability, the quality of the unsaturated three/dicarboxylic acids minor comonomer little list than unsaturated monocarboxylic acid
The quality of body is little, so can additionally mate other functions minor comonomer in high performance water-reducer component and collapsing, protecting come the guarantor to improve water reducer
Mould ability.
CN 105037647 A discloses a kind of preparation method of polycarboxylic admixture, belongs to cement water reducing agent field.
Additive of the present invention is by polymeric monomer methylpropenyl polyoxyethylene ether and maleic anhydride, passes through poly- in redox system
Close reaction, be simultaneously introduced thin base propanoic acid, hydroxyl ethyl ester and fumaric acid, in deionized water side chain is increased by polyreaction, simultaneously
Introduce side chain, so that molecular structure is formed and carry-SH, the comb-type structure of the hydrophilic functional group such as-OH ,-COOH.
CN 101786824 A discloses a kind of plastic retaining type polyether assemblage carboxylic acid high-performance water reducing agent and preparation method thereof, should
For building material field.This water reducer is in the presence of initiator, by unsaturated polyoxyalkyl ether monomer (A), unsaturation
Monocarboxylic acid and its derivatives monomer (B), unsaturated dicarboxylic acid and its derivatives monomer (C) and unsaturated sulfonic acid or its salt list
Body (D) copolymerization 2～8 hours in aqueous solution under 50～80 degree, are then cooled to 35～45 degree and are neutralized to pH with alkaline solution
=5～7 are obtained.
CN 103508696 A discloses a kind of Mud-resistant polycarboxylic acid water reducer, and it is made up of following components raw material：Allyl
Base class polyoxyethylene poly-oxygen propylene aether, component R, R1, R2, chain-transferring agent, initiator R3 and water, component R is maleic anhydride, methyl
One or more of sodium allylsulfonate, vinylacetate, itaconic acid, itaconic anhydride, fumaric acid；R1 is acrylic acid, methyl-prop
The mixture of one of olefin(e) acid or two kinds；R2 be ascorbic acid, sodium formaldehyde sulfoxylate, ferrous sulfate, stannous sulfate, sodium hypophosphite,
One or more of sodium sulfite, oxalic acid；Also disclose its preparation method.
Content of the invention
The technical problem to be solved is to provide a kind of poly- carboxylic of high-adaptability of total solids spatter property raw material preparation
Sour diminishing masterbatch, is divided by following each groups and is polymerized, raw material gross mass be 1000 parts, each group divide including：
Polyether macromonomer：350～360；
Unsaturated carboxylic acid：13.2～22.2；
Unsaturated acid anhydride：7.0～15.0；
Solid kind oxidant：2.0～5.0；
Solid kind reducing agent：0.6～5.0；
Solid kind chain-transferring agent：3.0～5.0；
Water：Remaining.
Described polyether macromonomer is allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, prenol polyoxy second
Alkene ether, one or more compositions of vinyl butyl ether polyoxyethylene ether；In view of unsaturated acid anhydride and unsaturation in synthetic system
High unit carboxylic acidss minor comonomer reactivity relatively low it is necessary to suitably weaken the reactivity of polyether macromonomer, with covert improve little
The reactivity ratio of monomer, described polyether macromonomer judges from the balanced angle of reactivity ratio, preferably allyl polyethenoxy ether,
One or two compositions of methyl allyl polyoxyethylene ether；
Described polyether macromonomer judges from the angle of high-adaptability, preferably methyl allyl polyoxyethylene ether；
Described solid kind oxidant is sodium dichromate, potassium permanganate, Ammonium persulfate., potassium peroxydisulfate, SODIUM PERCARBONATE, excessively boron
Sour sodium, one or more compositions of potassium perborate；It is solid that described solid kind oxidant is preferably the non-volatile zest of nonstaining property
Body class oxidant, i.e. one or more compositions of SODIUM PERCARBONATE, Dexol, potassium perborate；
Described solid kind chain-transferring agent is methacrylic sulfonic acids sodium, one or two compositions of sodium hypophosphite；Described
Solid kind chain-transferring agent be preferably nonstaining property non-volatile zest solid kind chain-transferring agent, that is, methacrylic sulfonic acids sodium,
One or two compositions of sodium hypophosphite；
Described solid kind reducing agent is sodium dithionite, sodium formaldehyde sulphoxylate, ascorbic acid, bisulfite
Sodium, sodium pyrosulfite, Dextrose Monohydrate, one or more compositions of Fructose；Described solid kind reducing agent is preferably solid kind
Weak reductant, i.e. one or more compositions of sodium sulfite, sodium pyrosulfite, Dextrose Monohydrate, Fructose；Described solid kind
Reducing agent be preferably nonstaining property non-volatile zest solid kind weak reductant, that is, Dextrose Monohydrate, Fructose one or two
Composition；
Initiator is the water solution mixture of solid kind chain-transferring agent and solid kind reducing agent.
Described unsaturated carboxylic acid includes unsaturated monocarboxylic acid, i.e. acrylic acid；Undersaturated dicarboxylic acids, i.e. clothing health
Acid, fumaric acid；Unsaturated tricarboxylic acid, i.e. equisetic acid；It is preferably nonstaining property non-volatile zest solid kind unsaturation polynary
Carboxylic acidss minor comonomer, i.e. one or two compositions of itaconic acid, equisetic acid；
Described unsaturated acid anhydride is maleic anhydride, itaconic anhydride, phthalic anhydride, trimellitic anhydride, dimethyl
One or more compositions of maleic anhydride and succinic anhydrides；It is preferably the non-volatile zest solid of the preferable nonstaining property of water solublity
Class unsaturated acids anhydride minor comonomer, i.e. one or more compositions of maleic anhydride, itaconic anhydride, dimethyl maleic anhydride.
The preparation method of the high-adaptability polycarboxylate water-reducer masterbatch of total solids spatter property raw material preparation of the present invention, including
Following operating procedure：
Polyether macromonomer is placed in reaction vessel, continuously stirred, until solution no obvious bulk or sheet material；
Solid kind oxidant is placed in and dissolves completely in polyether macromonomer solution, then 10min domestic demand sequentially adds
Initiator and minor comonomer solution, minor comonomer solution time for adding is 3～4h, and initiator lags behind minor comonomer solution 10～20min
After drip；Described minor comonomer solution is the aqueous solution of unsaturated carboxylic acid and unsaturated acid anhydride；
Do not open cooling water circulation, and be not added with liquid caustic soda neutralization, can release after being placed in 10～15h in reactor.
The state of considered critical raw material of the present invention and abnormal smells from the patient, being satisfied with clean manufacturing in storage and ventilation equipment will
Ask, its design concept is to improve carboxyl density to improve the initial dispersion of Water-reducing Admixtures To Cements slurry, after mating in component
The anhydrides minor comonomer of phase hydrolysis release carboxyl, with the synchronous dispersion retentivity improving cement slurry.
The invention has the beneficial effects as follows：
1. the use of unsaturated dicarboxylic acid minor comonomer-itaconic acid and unsaturated tricarboxylic acid minor comonomer-equisetic acid, improves
The carboxyl density of water reducer, using the longer weak reduction of the relatively low methyl allyl polyoxyethylene ether of reactivity ratio and half-life
Agent, to guarantee the polymerization effect of itaconic acid, equisetic acid.
2., under equal anchoring absorbability, in synthetic ratio design, unsaturated two/tricarboxylic acid minor comonomer quality compares insatiable hunger
Little with the quality of monocarboxylic acid minor comonomer, therefore in synthetic ratio, still have the unsaturated acids of components do match later stage hydrolysis release carboxylate radical
Anhydride minor comonomer, polyether macromonomer consumption design simultaneously can be bigger than normal, and a chain density is relatively higher, and water reducer is protected the ability of collapsing and protected
Card.
Specific embodiment
Below by example, the present invention will be further elaborated, and the description below is not only for explaining the present invention, right
Content is defined.
Embodiment 1
A kind of total solids spatter property raw material high-adaptability polycarboxylate water-reducer masterbatch, this water reducer is by by mass percentage
Following each groups divide and be polymerized, raw material gross mass is 1000, and each component and technological parameter are as follows：
Bed material：The isopentenol polyoxyethylene ether of 2400 molecular weight：352, water：200；
Oxidizing agent solution：SODIUM PERCARBONATE：5, water：5；
Initiator, minor comonomer solution is sequentially added in 10min after oxidizing agent solution addition；
Initiator：Methacrylic sulfonic acids sodium：3.7, ascorbic acid：0.85, water：120；
Minor comonomer solution：Itaconic acid：22.2, maleic anhydride：8, water：50；
Initiator time for adding：3.5h；
Minor comonomer solution time for adding 3.0h；
Moisturizing：233.25.
Insulation 10h releases reactor.
Embodiment 2
Bed material：The allyl polyethenoxy ether of 2400 molecular weight：355, water：220；
Oxidizing agent solution：Dexol：3.8, water：10；
Initiator, minor comonomer solution is sequentially added in 10min after oxidizing agent solution addition；
Initiator：Sodium hypophosphite：4.65, Dextrose Monohydrate：5, water：120；
Minor comonomer solution：Equisetic acid：15.7, itaconic anhydride：10.2, water：50；
Initiator time for adding：4.0h；
Minor comonomer solution time for adding 3.5h；
Moisturizing：205.65.
Insulation 15h releases reactor.
Embodiment 3
Bed material：The methyl allyl polyoxyethylene ether of 2400 molecular weight：357, water：250；
Oxidizing agent solution：Potassium perborate：2.5, water：15；
Initiator, minor comonomer solution is sequentially added in 10min after oxidizing agent solution addition；
Initiator：Sodium hypophosphite：5.0, Fructose：4.7, water：120；
Minor comonomer solution：Itaconic acid：18.6, dimethyl maleic anhydride：10.5, water：50；
Initiator time for adding：3.5h；
Minor comonomer solution time for adding 3.0h；
Moisturizing：166.7.
Insulation 12h releases reactor.
Embodiment 4
Bed material：The methyl allyl polyoxyethylene ether of 2400 molecular weight：350, water：250；
Oxidizing agent solution：Potassium perborate：4.2, water：12；
Initiator, minor comonomer solution is sequentially added in 10min after oxidizing agent solution addition；
Initiator：Methacrylic sulfonic acids sodium：4.2, Dextrose Monohydrate：2.7, sodium sulfite：2.2, water：120；
Minor comonomer solution：Equisetic acid：12.7, maleic anhydride：13.2, water：50；
Initiator time for adding：3.5h；
Minor comonomer solution time for adding 3.0h；
Moisturizing：178.8.
Insulation 15h releases reactor.
The high-adaptability polycarboxylate water-reducer masterbatch of total solids spatter property raw material preparation
Respectively in test examples detailed above the preparation of total solids spatter property raw material high-adaptability polycarboxylate superplasticizer mother liquor and general
Pulp flowage under the equal consumption of logical polycarboxylate superplasticizer mother liquor and through when mobility.Cement used by experiment is Hua Xin
42.5 ordinary portland cements, Ge Zhou Ba 42.5 ordinary portland cement, capital orchid 42.5 ordinary portland cements, with reference to GB/8076-2008《Concrete is additional
Agent》Test pulp flowage.
The new pulp flowage impact to China of the different water reducer of table 1
The different water reducer of table 2 affects on Ge Zhou Ba pulp flowage
The different water reducer of table 3 is on capital orchid pulp flowage impact
By table 1-3 as shown by data, ordinary water-reducing agent is directed to Hua Xin, Ge Zhou Ba, capital orchid cement show different initial,
Through when mobility, in the case of the orchid cement of its Zhong jing, no mobility；Example 1,2,3 water reducer is directed to Hua Xin, Ge Zhou Ba, capital orchid
Cement shows metastable mobile performance, in the case of its Zhong jing orchid cement, still possesses the flowing that can be satisfied with service behaviour
Property.In sum, under different cement, example 1,2,3 water-reducing rates and function of slump protection relatively stable, the strong adaptability of performance；Study carefully it former
High-adaptability polycarboxylate water-reducer recipe ingredient because being the preparation of solid cleaning raw material is designed with unsaturated polybasic carboxylic acid
Its slump retaining and stability are increased with the amount of other minor comonomers of having more than needed.
Claims (5)
1. a kind of high-adaptability polycarboxylate water-reducer masterbatch of total solids spatter property raw material preparation, by the conjunction of following each group segregations
Become, raw material gross mass be 1000 parts, each group divide including：
Polyether macromonomer：350~360；
Unsaturated carboxylic acid：13.2~22.2；
Unsaturated acid anhydride：7.0~15.0；
Solid kind oxidant：2.0~5.0；
Solid kind reducing agent：0.6~5.0；
Solid kind chain-transferring agent：3.0~5.0；
Water：Remaining；
Described polyether macromonomer be allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, isopentenol polyoxyethylene ether,
One or more compositions of vinyl butyl ether polyoxyethylene ether；
Described unsaturated carboxylic acid includes acrylic acid, itaconic acid, fumaric acid or equisetic acid；
Described unsaturated acid anhydride is maleic anhydride, itaconic anhydride, phthalic anhydride, trimellitic anhydride, dimethyl Malaysia
One or more compositions of anhydride and succinic anhydrides.
2. high-adaptability polycarboxylate water-reducer masterbatch according to claim 1 is it is characterised in that described solid kind aoxidizes
Agent is sodium dichromate, potassium permanganate, Ammonium persulfate., potassium peroxydisulfate, SODIUM PERCARBONATE, Dexol, one kind of potassium perborate or several
Plant composition.
3. high-adaptability polycarboxylate water-reducer masterbatch according to claim 1 is it is characterised in that described solid kind chain turns
Shifting agent is methacrylic sulfonic acids sodium, one or two compositions of sodium hypophosphite.
4. high-adaptability polycarboxylate water-reducer masterbatch according to claim 1 is it is characterised in that described solid kind reduces
Agent be sodium dithionite, sodium formaldehyde sulphoxylate, ascorbic acid, sodium sulfite, sodium pyrosulfite, Dextrose Monohydrate,
One or more compositions of Fructose.
5. the preparation side of the high-adaptability polycarboxylate water-reducer masterbatch of total solids spatter property raw material preparation described in claim 1
Method is it is characterised in that include following operating procedure：
Polyether macromonomer is placed in reaction vessel, continuously stirred, until solution no obvious bulk or sheet material；
Solid kind oxidant is placed in and dissolves completely in polyether macromonomer solution, then 10min domestic demand sequentially adds initiation
Agent and minor comonomer solution, minor comonomer solution time for adding is 3 ~ 4h, and initiator lags behind Deca after minor comonomer solution 10 ~ 20min
Complete；Described minor comonomer solution is the aqueous solution of unsaturated carboxylic acid and unsaturated acid anhydride；
Do not open cooling water circulation, and be not added with liquid caustic soda neutralization, can release after being placed in 10 ~ 15h in reactor.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592264A (en) * | 2020-05-26 | 2020-08-28 | 重庆三圣实业股份有限公司 | Dicarboxyl sulfonic acid group polycarboxylic acid water reducing agent and preparation method thereof |
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Application publication date: 20170215 |