CN106746873A - The preparation method of powdery polycarboxylic-acid high-performance water reducing agent - Google Patents
The preparation method of powdery polycarboxylic-acid high-performance water reducing agent Download PDFInfo
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- CN106746873A CN106746873A CN201710127467.6A CN201710127467A CN106746873A CN 106746873 A CN106746873 A CN 106746873A CN 201710127467 A CN201710127467 A CN 201710127467A CN 106746873 A CN106746873 A CN 106746873A
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0042—Powdery mixtures
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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
- C04B2103/302—Water reducers
Abstract
The invention discloses a kind of powdery polycarboxylic-acid high-performance water reducing agent and preparation method thereof, preparation method includes step：(1) preparation of glycerol maleate ester：To maleic anhydride, glycerine and catalyst that metering is added in reactor, separate water layer and lower the temperature；(2) preparation of molten state polycarboxylate high performance water-reducing agent：The polyether monomer of metering is added in reactor, stirring melts, and adds unsaturated sulfonic acid salt and oil-soluble initiator stirring and dissolving；Then water soluble starter, chain-transferring agent and acrylic or methacrylic acid are made into mixed solution to add；(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to freezing crusher, and low-temperature grinding is carried out at 20~40 DEG C, and powdery polycarboxylic-acid high-performance water reducing agent is obtained.The present invention can according to actual needs prepare any concentration solution, with good diminishing dispersion effect, and without heat drying or separate the postprocessing working procedures such as solvent, and cost of transportation is lower.
Description
Technical field
The invention belongs to cement water reducing agent field, and in particular to a kind of powdery polycarboxylic-acid high-performance water reducing agent and its
Preparation method.
Background technology
With the rise of the Large Infrastructure Projects such as China's nuclear power, water conservancy, bridge, tunnel, especially state-owned railroads passenger traffic is special
The extensive implementation of gauze engineering, the market demand sustainable growth to poly carboxylic acid series water reducer.With traditional high efficiency water reducing agent phase
Than poly carboxylic acid series water reducer has turned into concrete property high with premium properties such as its high water reducing rate, low slump loss, Lower alrali contents
The critical material of energyization.
Poly carboxylic acid series water reducer in the market is generally 10~50% fluid product, due to its superior performance, more
It is used in various key projects come more.But often due to engineering construction place farther out, job site place it is limited, cause to deposit
Storage, cost of transportation constantly increase, so development high concentration or powdered polycarboxylic acids product are to reduce cost of transportation and promote poly-
The widely used essential condition of carboxylic acid water reducing agent.The wide popularization and application of dry powder and mortar, also to solid poly carboxylic acid series water reducer
Production application propose active demand.Powder poly carboxylic acid series water reducer in the market is generally to be obtained by spray drying process
Arrive, but be diluted to liquid, performance has declined compared with the liquid poly carboxylic acid series water reducer with concentration, and this is mainly poly-
There is partial cross-linked causing after being heated in carboxylic acid water reducing agent.If expecting that the poly carboxylic acid series water reducer powder of excellent performance is produced
Product, can not only destroy operation under conditions of poly carboxylic acid series water reducer structure by the way of low temperature.
Therefore, powdery polycarboxylic-acid high-performance water reducing agent is researched and developed, undoubtedly for accelerating poly carboxylic acid series water reducer row
The development of industry, popularization poly carboxylic acid series water reducer application are extremely important.
The content of the invention
For problems of the prior art, the present invention provide a kind of powdery polycarboxylic-acid high-performance water reducing agent and its
Preparation method, safe preparation process environmental protection, obtained water reducer water-reducing property is good.
A kind of powdery polycarboxylic-acid high-performance water reducing agent, the parts by weight of raw material are：
The glycerine is (2.2~2.8) with the mol ratio of maleic anhydride: 1.0.
The catalyst is p-methyl benzenesulfonic acid or sulfamic acid, and consumption is the 1.5~3% of glycerin weight number.
The polyether monomer is methyl allyl alcohol polyoxyethylene ether, the methallyl alcohol polyoxy second of molecular weight 1000~5000
One kind in alkene polyethenoxy ether, isopentenol polyoxyethylene ether, prenol polyoxyethylene poly-oxygen propylene aether.
During the unsaturated sulfonic acid salt is including allylsulfonate, methallylsulfonic acid salt, styrene sulfonate etc.
The mixture of one or more.
The oil-soluble initiator is azodiisobutyronitrile, ABVN, azo-bis-iso-dimethyl, peroxidating
One kind in benzoyl, the benzoyl peroxide tert-butyl ester, methyl ethyl ketone peroxide, the water soluble starter is ammonium persulfate, mistake
One kind in sodium sulphate and potassium peroxydisulfate.
Described chain-transferring agent is hydrophobic chain transfer agent, including butyl mercaptan, spicy thioalcohol, decyl mercaptan, lauryl mercaptan, ten
Six alkyl hydrosulfides, Stearyl mercaptan, 2 mercaptopropionic acid monooctyl ester, 3- mercaptopropionic acids monooctyl ester, thio glycolic monooctyl ester, sulfydryl second
Acid -2- Octyl Nitrites, may be used singly or in combin two kinds or more.
The invention further relates to a kind of preparation method of powdery polycarboxylic-acid high-performance water reducing agent, comprise the following steps：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle, maleic anhydride, glycerine and the catalyst of metering are added, 110~150 DEG C are warming up under agitation, be stirred at reflux 3~6h,
Water layer is separated with water knockout drum and be cooled to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：The polyether monomer of metering is added in reactor, stirring is molten
Solution, adds unsaturated sulfonic acid salt and oil-soluble initiator stirring and dissolving；Then by water soluble starter, chain-transferring agent and propylene
Acid or methacrylic acid are made into mixed solution, and are dripped off with constant flow pump in 2~4h；Follow-up continuation of insurance 2~4h of temperature is dripped off, meter is added
The powder alkali of amount stirs；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine, carries out low-temperature grinding at -20~-40 DEG C, that is, the powdery polycarboxylic-acid high-performance that fineness is 100~200 mesh is obtained and subtracts
Aqua.
The initiator feed postition disposably puts into reactor for oil-soluble initiator as bed material, and water solubility triggers
Agent is dissolved in unsaturated carboxylic acid and is slowly dropped in reactor.
The inventive method has the advantages that compared with prior art：
(1) the low entraining type powdery polycarboxylic-acid water reducer prepared using the present invention, can avoid spray drying treatment
The problems such as caused chemical side reactions or wall built-up calcination, the abundant method for preparing powdery polycarboxylic-acid water reducer.
(2) safe preparation process is environmentally friendly, solvent-free murder by poisoning, cleanliness without any pollution, reaction raw materials used are simply common, synthesize
Cheng Wuxu nitrogen is protected, and greatly reduces production cost.
(3) synthesis technique is simple efficiently, safety and environmental protection is pollution-free, production cost and energy consumption is low, convenient transportation the advantages of, have
Beneficial to industrial application, with good economic benefit and social benefit.
(4) preparing gained water reducer has excellent diminishing dispersion effect, remains to show preferably under compared with low-dosage
Mobility and holding capacity, and cement to different cultivars shows very strong adaptability.Additionally, water reducer Product Status are steady
It is fixed, deposited under low temperature and do not crystallized, and performance is unaffected after low-temperature storage.
Specific embodiment
Describe embodiments of the present invention in detail with specific embodiment below, whereby to the present invention how application technology hand
Section solves technical problem, and reaches the implementation process of technique effect and can fully understand and implement according to this.
Embodiment 1：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 167.6kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 346.0kg glycerine and
5.2kg p-methyl benzenesulfonic acid, is warming up to 140~150 DEG C under agitation, is stirred at reflux 3~3.5h, separates water layer with water knockout drum and drops
Temperature is to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 3775kg isopentenol polyoxyethylene ether (molecules
And 124.2kg methylpropene sodium sulfonates 2400), stirring melts amount, adds 34.0kg benzoyl peroxide stirring and dissolvings；Then
14.6kg sodium peroxydisulfates, 19.5kg 3- mercaptopropionic acids monooctyl esters and 452.8kg acrylic acid are made into mixed solution, and in 3.5~4h
Interior constant flow pump is dripped off；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 61.1kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 2：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 384.2kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 865.7kg glycerine and
13.0kg p-methyl benzenesulfonic acid, is warming up to 110~120 DEG C under agitation, is stirred at reflux 5~5.5h, and water layer is separated simultaneously with water knockout drum
It is cooled to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：2805kg methyl allyl alcohol polyoxyethylene ethers are added (to divide
And 168.4kg ALSs 1200), stirring melts son amount, adds 33.9kg azodiisobutyronitrile stirring and dissolvings；Then
14.5kg ammonium persulfates, 24.1kg 2 mercaptopropionic acids monooctyl ester and 605.7kg acrylic acid are made into mixed solution, and in 3.5~4h
Interior constant flow pump is dripped off；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 85.5kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 3：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 324.2kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 730.3kg glycerine and
14.6kg sulfamic acids, are warming up to 110~120 DEG C under agitation, are stirred at reflux 5~5.5h, separate water layer with water knockout drum and drop
Temperature is to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 2850kg isopentenol polyoxyethylene ether (molecules
And 187.7kg methylpropene sodium sulfonates 1200), stirring melts amount, adds the stirring of 33.7kg azo-bis-iso-dimethyls molten
Solution；Then 14.5kg potassium peroxydisulfates, the thio glycolic monooctyl esters of 29.0kg and 715.1kg methacrylic acids are made into mixed solution,
And dripped off with constant flow pump in 3.5~4h；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 100.9kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 4：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 100.8kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 246.2kg glycerine and
3.7kg p-methyl benzenesulfonic acid, is warming up to 140~150 DEG C under agitation, is stirred at reflux 3~3.5h, separates water layer with water knockout drum and drops
Temperature is to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 4208kg isopentenol polyoxyethylene ether (molecules
And 84.2kg ALSs 3600), stirring melts amount, adds 34.2kg benzoyl peroxide stirring and dissolvings；Then will
14.7kg sodium peroxydisulfates, 19.5kg spicy thioalcohols and 252.5kg acrylic acid are made into mixed solution, and constant flow pump is used in 3.5~4h
Drip off；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 36.2kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 5：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 89.4kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 218.3kg glycerine and
4.4kg sulfamic acids, are warming up to 110~120 DEG C under agitation, are stirred at reflux 3~3.5h, separate water layer with water knockout drum and lower the temperature
To 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 4160kg isopentenol polyoxyethylene ether (molecules
And 107.2kg SSSs 4000), stirring melts amount, adds 34.1kg ABVN stirring and dissolvings；Then will
14.7kg potassium peroxydisulfates, 29.2kg butyl mercaptan and 299.6kg acrylic acid are made into mixed solution, and constant flow pump is used in 3.5~4h
Drip off；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 43.1kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 6：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 134.1kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 327.5kg glycerine and
8.2kg sulfamic acids, are warming up to 110~120 DEG C under agitation, are stirred at reflux 3~3.5h, separate water layer with water knockout drum and lower the temperature
To 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 3758kg prenol polyoxyethylene polyoxy third
Alkene ether (molecular weight 2400) and 161.3kg SSSs, stirring melt, and add the stirring of 34.0kg benzoyl peroxides molten
Solution；Then 14.6kg potassium peroxydisulfates, 24.3kg decyl mercaptans and 471.4kg methacrylic acids are made into mixed solution, and 3.5~
The interior constant flow pumps of 4h are dripped off；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 66.6kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 7：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 67.2kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 176.8kg glycerine and
2.7kg p-methyl benzenesulfonic acid, is warming up to 140~150 DEG C under agitation, is stirred at reflux 3~3.5h, separates water layer with water knockout drum and drops
Temperature is to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 3945kg methallyl alcohol polyoxyethylene polyoxies
Propylene ether (molecular weight 2400) and 130.0kg methylpropene sodium sulfonates, stirring melt, and add 29.1kg benzoyl peroxides and stir
Mix dissolving；Then 19.4kg ammonium persulfates, the thio glycolic monooctyl esters of 24.3kg and 532.8kg acrylic acid are made into mixed solution,
And dripped off with constant flow pump in 3.5~4h；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 72.7kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 8：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 114.4kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 300.8kg glycerine and
6.0kg p-methyl benzenesulfonic acid, is warming up to 110~120 DEG C under agitation, is stirred at reflux 4~4.5h, separates water layer with water knockout drum and drops
Temperature is to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 3370kg isopentenol polyoxyethylene ether (molecules
And 205.0kg ALSs 1200), stirring melts amount, adds 24.1kg benzoyl peroxide tert-butyl ester stirring and dissolvings；
Then 23.9kg sodium peroxydisulfates, 38.5kg thioglycollic acid-2-ethyl hexyl esters and 808.6kg acrylic acid are made into mixed solution, and
Dripped off with constant flow pump in 3.5~4h；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 108.7kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Embodiment 9：
(1) preparation of glycerol maleate ester：To the reaction equipped with thermometer, stirring slurry, constant flow pump, condenser and water knockout drum
In kettle add 136.5kg maleic anhydrides, 70 DEG C are warming up under stirring, melted completely to bed material, add 281.8kg glycerine and
7.0kg sulfamic acids, are warming up to 140~150 DEG C under agitation, are stirred at reflux 3~3.5h, separate water layer with water knockout drum and lower the temperature
To 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：Add 3780kg isopentenol polyoxyethylene ether (molecules
And 162.2kg SSSs 2400), stirring melts amount, adds 24.2kg methyl ethyl ketone peroxide stirring and dissolvings；Then will
The thio glycolic monooctyl ester of 24.2kg ammonium persulfates, 27.5kg and 488.3kg methacrylic acids are made into mixed solution, and 3.5~
The interior constant flow pumps of 4h are dripped off；Follow-up continuation of insurance 2~2.5h of temperature is dripped off, adds 68.3kg powder alkali to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to Freezing smashing by utilidor
Machine low-temperature grinding, that is, be obtained white powder polycarboxylate high performance water-reducing agent.
Application Example 1：
Flowing degree of net paste of cement is with reference to standard GB/T/T 8077-2012《Methods for testing uniformity of concrete admixture》,
Three kinds of cement are respectively reference cement, the cement of crane woods PO 42.5 of Jiangsu He Lin Cement Co., Ltds product and Nanjing little Ye fields
The peaceful sheep PII52.5 cement of gold that Cement Co., Ltd produces；Liquid of the poly carboxylic acid series water reducer of contrast from Nanjing company
The product TX-50H and powder product PC-80 of Jiangsu factory, (weight with cement after rolling over admittedly is for 0.16% for the volume of water reducer
Benchmark meter), result of the test is shown in Table 1.
Table 1 mixes the flowing degree of net paste of cement after the present invention
From the result of table 1, powdery polycarboxylic-acid high-performance water reducing agent of the invention is substantially better than city in dispersive property
Powder control sample is sold, dispersiveness and dispersed holding capacity are basic with commercially available common liq polycarboxylate high performance water-reducing agent sample
Close, solid is melt-synthesized and freezing smashes and water reducer performance is not influenceed substantially.
Application Example 2：
With reference to standard GB/T 8076-2008《Concrete admixture》Relevant regulations are performed.Testing cement uses reference water
Mud, C: S: G=360: 836: 1024 in concrete mix, water reducer is mixes 0.2% admittedly, and adjustment water consumption makes newly to mix coagulation
Native initial slump is 210mm ± 10mm, and result of the test see the table below 2.
The concrete performance contrast of the different poly carboxylic acid series water reducers of table 2
From the result of table 2, water-reducing rate is reachable when the solid volume of powdery polycarboxylic-acid water reducer folding of the invention is 0.2%
More than 25%, water-reducing rate is approached with commercial liquid polycarboxylate high performance water-reducing agent and is higher than commercially available powder polycarboxylic acid series high-performance
Water reducer, fresh concrete slump 1h internal losses are smaller, with the characteristics of water-reducing rate is high and function of slump protection is good, to different larval instar
Compression strength also has no adverse effects.
Although the present invention is described by embodiment, embodiment is not used for limiting the present invention.Art technology
Personnel can make various modifications and improvement in the scope of spirit of the invention, the adjustment of such as component ratio or time range,
Effect after this adjustment is predictable, so it is same within protection scope of the present invention.Therefore protection of the invention
The protection domain that scope should be defined by the identical or equivalent technical characteristic of claims hereof is defined.
Claims (9)
1. a kind of powdery polycarboxylic-acid high-performance water reducing agent, it is characterised in that the parts by weight of raw material are：
2. powdery polycarboxylic-acid high-performance water reducing agent according to claim 1, it is characterised in that：The glycerine with it is described
The mol ratio of maleic anhydride is (2.2~2.8): 1.0.
3. powdery polycarboxylic-acid high-performance water reducing agent according to claim 1, it is characterised in that：The catalyst is right
Toluenesulfonic acid or sulfamic acid, consumption are the 1.5%~3% of the glycerin weight number.
4. powdery polycarboxylic-acid high-performance water reducing agent according to claim 1, it is characterised in that：The polyether monomer is
The methyl allyl alcohol polyoxyethylene ether of molecular weight 1000~5000, methallyl alcohol polyoxyethylene poly-oxygen propylene aether, prenol
One kind in APEO, prenol polyoxyethylene poly-oxygen propylene aether.
5. powdery polycarboxylic-acid high-performance water reducing agent according to claim 1, it is characterised in that：The unsaturated sulfonic acid
Salt includes one or more in allylsulfonate, methallylsulfonic acid salt, styrene sulfonate.
6. powdery polycarboxylic-acid high-performance water reducing agent according to claim 1, it is characterised in that：The oil-soluble triggers
Agent is azodiisobutyronitrile, ABVN, azo-bis-iso-dimethyl, benzoyl peroxide, benzoyl peroxide uncle
One kind in butyl ester, methyl ethyl ketone peroxide, the water soluble starter is in ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate
Kind.
7. powdery polycarboxylic-acid high-performance water reducing agent according to claim 1, it is characterised in that：The chain-transferring agent is
Hydrophobic chain transfer agent, including butyl mercaptan, spicy thioalcohol, decyl mercaptan, lauryl mercaptan, hexadecyl mercaptan, Stearyl mercaptan,
One kind or several in 2 mercaptopropionic acid monooctyl ester, 3- mercaptopropionic acids monooctyl ester, thio glycolic monooctyl ester, thioglycollic acid-2-ethyl hexyl ester
Kind.
8. in a kind of claim 1-7 any described powdery polycarboxylic-acid high-performance water reducing agent preparation method, its feature
It is to comprise the following steps：
(1) preparation of glycerol maleate ester：To maleic anhydride, glycerine and catalyst that metering is added in reactor, under agitation
110~150 DEG C are warming up to, 3~6h is stirred at reflux, water layer are separated and is cooled to 60~70 DEG C；
(2) preparation of molten state polycarboxylate high performance water-reducing agent：The polyether monomer of metering is added in reactor, stirring melts,
Add unsaturated sulfonic acid salt and oil-soluble initiator stirring and dissolving；Then by water soluble starter, chain-transferring agent and acrylic acid
Or methacrylic acid is made into mixed solution addition；Follow-up continuation of insurance 2~4h of temperature is added, adds the powder alkali of metering to stir；
(3) preparation of powdery polycarboxylic-acid high-performance water reducing agent：Molten product delivers to freezing crusher, at -20~-40 DEG C
Low-temperature grinding is carried out, prepared fineness is the powdery polycarboxylic-acid high-performance water reducing agent of 100~200 mesh.
9. the preparation method of powdery polycarboxylic-acid high-performance water reducing agent according to claim 8, it is characterised in that：It is described
Oil-soluble initiator disposably puts into reactor as bed material, and the water soluble starter is dissolved in unsaturated carboxylic acid and is slowly added dropwise
To in reactor；Water soluble starter, chain-transferring agent and acrylic or methacrylic acid are made into mixed solution, and in 2~4h
Interior constant flow pump is dripped off.
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| CN102775089A (en) * | 2012-08-21 | 2012-11-14 | 南京瑞迪高新技术有限公司 | Star polycarboxylic-acid high-performance water reducing agent and preparation method thereof |
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