CN108948284A - A kind of polyether ester modified polyether water-reducing agent and preparation method thereof - Google Patents
A kind of polyether ester modified polyether water-reducing agent and preparation method thereof Download PDFInfo
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- CN108948284A CN108948284A CN201810597011.0A CN201810597011A CN108948284A CN 108948284 A CN108948284 A CN 108948284A CN 201810597011 A CN201810597011 A CN 201810597011A CN 108948284 A CN108948284 A CN 108948284A
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- water
- reducing agent
- ether
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- agent
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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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
- C04B24/2658—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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 present invention provides a kind of anhydrous water-reducing agent and preparation method thereof, the water-reducing agent prepares in raw material while having used allyl alkene ether polymeric monomer and ether-ether class polymeric monomer, to combine the respective advantage that hydrophilic olefin polymerized monomer and more hydrophobic esters monomer influence water-reducing agent intensity, bleeding, simultaneously, relative to allyl ether series polymeric monomer is used alone, so that dehydration is more easier.It is dehydrated simultaneously using the supergravity dewatering device adaptable with water-reducing agent composition, the water-reducing agent dehydration rate of this method production is high, facilitates storage and transport, and prevented from caking during storage.In addition, the application is also it has been unexpectedly found that the water-reducing agent being prepared using the present processes, when being used for concrete, through when the slump vary less.
Description
Technical field
The present invention relates to technical field of fine, in particular to a kind of polyether ester modified polyether water-reducing agent and its preparation side
Method.
Background technique
Water-reducing agent is a kind of under conditions of maintaining concrete slump to be basically unchanged, and can be reduced the coagulation of mixing water amount
Native additive.
Polyethers water-reducing agent and poly carboxylic acid series water reducer are all water-reducing agent types more commonly used in recent years.Wherein polycarboxylic acids subtracts
Aqua is generally single by unsaturated carboxylic acid class, polyoxyalkylene alkyl hydrocarbon, esters of unsaturated carboxylic acids, the unsaturation containing sulfonic acid group using raw material
Body is prepared.CN1800076A discloses a kind of acrylic acid series multiple copolymer analog high efficiency water reducing agent, contains: acrylic acid or
100 parts of its derivative, 150~450 parts of polyoxyalkylene alkyl hydrocarbon, 10~80 parts of sulfonic acid system derivative, deionized water solvent 450~800
Part, 0.5~6 part of catalyst, 0.1~5 part of polymerization inhibitor, 5~30 parts of isopropanol chain-transferring agent, 0.5~5 part of initiator, NaOH is molten
The additional amount of liquid is that the pH value of product is made to reach 6~8.But method reaction process provided by the patent is difficult to control, water removal
Also difficult, in addition, bleeding does not refer to.Polypropylene alcohol ether: maleic anhydride: methylpropene sodium sulfonate: acrylamide: third
Olefin(e) acid -2- hydroxy methacrylate: initiator: water=25-40:3-6:1-6:0.5-4:1-5:0.5-4:100, the water-reducing agent
Little loss of slump, water-reducing rate are high, but its slump level is not high, and are dehydrated relatively difficult.
Summary of the invention
The purpose of the present invention is to provide a kind of anhydrous water-reducing agents and preparation method thereof, for this purpose, the application rational allocation
The composition of water-reducing agent, while being dehydrated using the supergravity dewatering device adaptable with water-reducing agent composition, this method production
Water-reducing agent dehydration rate is high, facilitates storage and transport, and prevented from caking during storage.In addition, the application is also against expectation
It was found that the water-reducing agent being prepared using the present processes, when being used for concrete, through when the slump vary less.
The application provides a kind of water-reducing agent first, which prepares in raw material while having used the big list of allyl alkene ether
Body and ether-ether class polymeric monomer, to combine hydrophilic olefin polymerized monomer and more hydrophobic esters monomer is strong for water-reducing agent
The respective advantage that degree, bleeding influence, meanwhile, relative to allyl ether series polymeric monomer is used alone, so that dehydration is more held
Easily.It is preferable to use allyl polyethenoxy ethers and methoxy poly (ethylene glycol) maleate, also exist using the advantages of maleate
Multiple carboxyls can be generated in the reaction in it, and the hydroxyl in these carboxyls and system can be relatively easy to crosslinking, to have
Conducive to the intensity for improving concrete.
It is furthermore preferred that a small amount of hydroxy silicon oil, such as methylol silicone oil can also be contained in the water-reducing agent.
More specifically, the application provides a kind of water-reducing agent, the raw material for preparing of the water-reducing agent includes: allyl polyethenoxy
Ether, methoxy poly (ethylene glycol) maleate, acrylic acid, 2- acryloyl group -2- methyl propane sulfonic acid, hydroxy silicon oil, oxidant, chain turn
Agent in shifting agent, reducing agent and alkali.
More specifically, the water-reducing agent prepares the raw material that raw material includes following parts by weight:
Allyl polyethenoxy ether 100-200, methoxy poly (ethylene glycol) maleate 10-20, acrylic acid 20-30,2- third
Enoyl- -2- methyl propane sulfonic acid 3-8, hydroxy silicon oil 1-2, oxidant 0.1-0.5, chain-transferring agent 0.1-0.5, reducing agent 0.1-
0.5 and alkali nertralizer.The dosage of alkali nertralizer is determining according to the pH of system after reaction, usually 1-10.
The oxidant can be peroxide, hydrogen peroxide etc., described peroxide such as peroxidation sulfuric acid potassium etc..
The chain-transferring agent can be thioacetic acid, mercaptopropionic acid, mercaptoethanol, lauryl mercaptan etc..
The reducing agent can be ascorbic acid, sodium sulfite, sodium hydrogensulfite etc..
The alkali nertralizer can be sodium hydroxide, sodium carbonate, sodium bicarbonate, preferably sodium hydroxide.
In addition the application provides a kind of preparation method of water-reducing agent, include the following steps:
Allyl polyethenoxy ether, methoxy poly (ethylene glycol) maleic acid are added into reactor for step 1, polymerization workshop section
Ester, 2- acryloyl group -2- methyl propane sulfonic acid, mixing form mixed liquor I, then oxidant is added in heating, then, are added dropwise by third
The mixed liquor I I of olefin(e) acid, chain-transferring agent and reducing agent composition after dripping, keeps the temperature 1-3 hours, is then added in alkali nertralizer
With obtain the diminishing agent solution of water content 30-40%；
Step 2 is dehydrated workshop section, the diminishing agent solution in step 1 is input in supergravity dewatering device and is dehydrated 0.5-5
Hour, obtain the water-reducing agent that solid content is 90% or more.
Preferably, the heating temperature in step 1 is 50-90 DEG C, and the holding temperature in step 2 is 60-90 DEG C of
Preferably, hydroxy silicon oil is also used in the mixed liquor preparation process of step 1.
Preferably, the structure of the supergravity dewatering device of step 2 is shell and the disk with discoid top surface
The parallel ring packing component in shape top surface, the heating layer on the shell inner surface layer, is located at the housing bottom surface at shaft
Semi-permeable film layer on the heating layer is passed into the hollow position of ring packing component across the discoid end face center
Water-reducing agent stoste outflow pipe, the water out positioned at the water-reducing agent outlet of shell two sides and positioned at lower part of the housing, the shaft prolong circle
The center of plate-like top surface is perpendicular to the discoid top surface, and the lower end of the centre bore of upper part and ring packing component
It is sealedly and fixedly connected, and the ring packing component can be driven to axially move, the ring packing component is by porous material system
At the water-reducing agent and water energy are enough pierced by from the hole of ring packing component under the influence of centrifugal force, the semipermeable membrane
Hole on layer can allow for hydrone to pass through, but diminishing agent molecule cannot be allowed to pass through.
It is further preferred that the water-reducing agent stoste outflow pipe of supergravity dewatering device is equipped with heating element, the water-reducing agent exists
60-90 DEG C, preferably 65-80 DEG C are pre-heated to before into supergravity dewatering device.In addition preferred, the ring packing component
Centre bore upper end on there is an annular lid, the ring cover body can cover the upper port of ring packing component and with subtract
There are gaps between aqua stoste outflow pipe.
It is also preferred that the revolving speed of the supergravity dewatering device is 500r/min-3000r/min.
In addition, the dehydration workshop section further include supergravity dewatering device dehydration after further progress vacuumize dehydration, pumping
The vacuum degree of vacuum is 0.095-0.1MPa, and temperature is 50-60 DEG C of
It, can be by the water-reducing agent for convenient transportation；Cooling slice.
The material of the filler component is the porous materials such as wire packing, metal foam filler, filling material of polymers.
The semipermeable membrane with a thickness of 0.1mm-10mm, material is cellulose acetate, polyamide, and composite membrane etc. is optional
Selecting property penetrates the film of water.
Detailed description of the invention
Fig. 1 is the schematic diagram of a specific embodiment of supergravity dewatering device of the present invention；
Fig. 2 is the schematic diagram of another specific embodiment of supergravity dewatering device of the present invention.
Description of symbols:
1, water-reducing agent stoste outflow pipe；
2, shell；
3, water-reducing agent exports；
4, semi-permeable film layer；
5, water out；
6, shaft；
7, ring packing component；
8, heating layer；
9, annular lid.
Specific embodiment
Invention is further explained combined with specific embodiments below, and the present invention is not limited to following case study on implementation.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, can obtain from commercial channels.
Embodiment 1
Allyl polyethenoxy ether, methoxy poly (ethylene glycol) maleic acid are added into reactor for step 1, polymerization workshop section
Ester, 2- acryloyl group -2- methyl propane sulfonic acid, mixing form mixed liquor I, then oxidant is added in heating, then, are added dropwise by third
The mixed liquor I I of olefin(e) acid, chain-transferring agent and reducing agent composition after dripping, keeps the temperature 1-3 hours, is then added in alkali nertralizer
With obtain the diminishing agent solution of water content 30-40%；
Step 2 is dehydrated workshop section, the diminishing agent solution in step 1 is input in supergravity dewatering device and is dehydrated 0.5-5
Hour, obtain the water-reducing agent that solid content is 90% or more.
Preferably, the heating temperature in step 1 is 50-90 DEG C, and the holding temperature in step 2 is 60-90 DEG C of
Allyl polyethenoxy ether 100-200, methoxy poly (ethylene glycol) maleate 10-20, acrylic acid 20-30,2- third
Enoyl- -2- methyl propane sulfonic acid 3-8, hydroxy silicon oil 1-2, oxidant 0.1-0.5, chain-transferring agent 0.1-0.5, reducing agent 0.1-
0.5 and alkali nertralizer.The dosage of alkali nertralizer is determining according to the pH of system after reaction, usually 1-10
Water and HPEG, methoxy poly (ethylene glycol) maleate, 2- acryloyl group-are added into the reactor with blender
2- methyl propane sulfonic acid, stirring and dissolving obtain mixed liquor I；Logical nitrogen protection, is heated to 60 DEG C, persulfuric acid is added in mixed liquor 1
Ammonium continues that the mixed liquor I I being made of acrylic acid aqueous solution, thioacetic acid and ascorbic acid, time for adding is added dropwise after mixing evenly
For 3h；After dripping, 2h is kept the temperature, sodium hydroxide, which is then added, makes the PH=6 of solution, and can be prepared by solid content is 30%-40%
Diminishing agent solution.The water in water-reducing agent finally is removed using gravity Method, the rotor speed of selected centrifuge is 500r/min,
60 DEG C of preparation temperature, dewatering time 4h, Fillers selection foam metal porous aggregate, semipermeable membrane with a thickness of 2mm, material is
PA membrane, final vacuum freeze drying, the solid content that water-reducing agent is made is 95.2%.In the reaction of the embodiment, allyl
Polyoxyethylene ether 100-200, methoxy poly (ethylene glycol) maleate 10-20, acrylic acid 20-30,2- acryloyl group -2- methyl-prop
Sulfonic acid 3-8, ammonium persulfate 0.1-0.5, thioacetic acid 0.1-0.5, ascorbic acid 0.1-0.5 amount ratio be 150:15:25:5:
0.2:0.2:0.3.
Embodiment 2
Other conditions are same as Example 1, the difference is that being also added into the preparation process of mixed liquor I and allyl
The hydroxy silicon oil of polyoxyethylene ether weight ratio 0.5:150.
Embodiment 3
Other conditions are same as Example 1, the difference is that being also added into the preparation process of mixed liquor I and allyl
The hydroxy silicon oil of polyoxyethylene ether weight ratio 1:150.
Embodiment 4
Other conditions are same as Example 1, the difference is that allyl polyethenoxy ether in the preparation process of mixed liquor I
With methoxy poly (ethylene glycol) maleate weight ratio 5:150.
Embodiment 5
Other conditions are same as Example 1, the difference is that being added without 2- acryloyl in the preparation process of mixed liquor I
Base -2- methyl propane sulfonic acid.
Comparative example 1
Other conditions are same as Example 1, the difference is that being added without the poly- second of methoxyl group in the preparation process of mixed liquor I
Glycol maleate.
Comparative example 2
Other conditions are same as Example 1, the difference is that allyl polyethenoxy ether in the preparation process of mixed liquor I
Weight ratio with methoxy poly (ethylene glycol) maleate is 1:1.
Table 1: water-reducing agent of the present invention and comparative example water-reducing agent water content and performance are compared
2 concrete slump of table and bleeding results of property
Claims (10)
1. a kind of water-reducing agent, the water-reducing agent prepares in raw material while having used allyl alkene ether polymeric monomer and the big list of ether-ether class
Body.
2. water-reducing agent described in claim 1, the water-reducing agent prepares in raw material while having used allyl polyethenoxy ether
With methoxy poly (ethylene glycol) maleate.
3. water-reducing agent as claimed in claim 2, preparing for the water-reducing agent also contains a small amount of hydroxy silicon oil in raw material.
4. the raw material for preparing of water-reducing agent as claimed in claim 3, the water-reducing agent includes: allyl polyethenoxy ether, methoxyl group
PEGMa polyethylene glycol maleate, acrylic acid, 2- acryloyl group -2- methyl propane sulfonic acid, hydroxy silicon oil, oxidant, chain-transferring agent, reduction
Agent and alkali nertralizer.
5. water-reducing agent described in any one of aforementioned claim, the water-reducing agent prepare the original that raw material includes following parts by weight
Material:
Allyl polyethenoxy ether 100-200, methoxy poly (ethylene glycol) maleate 10-20, acrylic acid 20-30,2- acryloyl
Base -2- methyl propane sulfonic acid 3-8, hydroxy silicon oil 1-2, oxidant 0.1-0.5, chain-transferring agent 0.1-0.5, reducing agent 0.1-0.5 and
Alkali nertralizer.
6. a kind of preparation method of water-reducing agent, includes the following steps:
Allyl polyethenoxy ether, methoxy poly (ethylene glycol) maleate, 2- are added into reactor for step 1, polymerization workshop section
Acryloyl group -2- methyl propane sulfonic acid, mixing, formed mixed liquor I, heating, oxidant is then added, then, be added dropwise by acrylic acid,
The mixed liquor I I of chain-transferring agent and reducing agent composition, after dripping, keeps the temperature 1-3 hours, and alkali nertralizer is then added and neutralizes, must contain
The diminishing agent solution of water 30-40%；
Step 2 is dehydrated workshop section, and it is small that the diminishing agent solution in step 1 is input to dehydration 0.5-5 in supergravity dewatering device
When, obtain the water-reducing agent that solid content is 90% or more.
7. preparation method as claimed in claim 6, wherein the heating temperature in step 1 is 50-90 DEG C, the heat preservation in step 2
Temperature is 60-90 DEG C, it is preferable that also uses hydroxy silicon oil in the preparation process of mixed liquor I in step 1.
8. the described in any item preparation methods of claim 6-7, wherein the structure of the supergravity dewatering device of step 2 includes:
Shell with discoid top surface, shaft, is located at table in the shell at the ring packing component parallel with the discoid top surface
Heating layer in surface layer, passes through the discoid end face center at the semi-transparent film layer on heating layer described in the housing bottom surface
It is passed into the water-reducing agent stoste outflow pipe of the hollow position of ring packing component, the water-reducing agent positioned at shell two sides exports and is located at
The water out of lower part of the housing, the shaft prolongs the center of discoid top surface perpendicular to the discoid top surface, and upper part
It is sealedly and fixedly connected with the lower end of the centre bore of ring packing component, and the ring packing component can be driven to make axial fortune
Dynamic, the ring packing component is made of porous materials, and the water-reducing agent and water energy are enough filled out from annular under the influence of centrifugal force
Expect to be pierced by the hole of component, the hole in the semi-transparent film layer can allow for hydrone to pass through, but cannot allow water-reducing agent point
Son passes through.
9. the water-reducing agent stoste outflow pipe of preparation method according to any one of claims 8, the supergravity dewatering device is equipped with heating
Component, the water-reducing agent are pre-heated to 60-90 DEG C, preferably 65-80 DEG C before entering supergravity dewatering device.
10. preparation method as claimed in claim 9, there is a ring cover on the upper end of the centre bore of the ring packing component
Body, which can cover the upper port of ring packing component and there are gaps between water-reducing agent stoste outflow pipe.
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| CN113563540A (en) * | 2021-07-31 | 2021-10-29 | 广东科隆智谷新材料股份有限公司 | Method for synthesizing polycarboxylate superplasticizer by using acrylic acid and hydroxyl silicone oil ester |
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