CN116515045A - Preparation method of slice type polycarboxylate superplasticizer - Google Patents
Preparation method of slice type polycarboxylate superplasticizer Download PDFInfo
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- CN116515045A CN116515045A CN202310505000.6A CN202310505000A CN116515045A CN 116515045 A CN116515045 A CN 116515045A CN 202310505000 A CN202310505000 A CN 202310505000A CN 116515045 A CN116515045 A CN 116515045A
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- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000008030 superplasticizer Substances 0.000 title claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000011282 treatment Methods 0.000 claims abstract description 31
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 30
- 229920000570 polyether Polymers 0.000 claims abstract description 30
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 27
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- 239000013543 active substance Substances 0.000 claims abstract description 9
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 238000001816 cooling Methods 0.000 claims description 23
- 238000006116 polymerization reaction Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 13
- 230000008020 evaporation Effects 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 5
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 5
- 239000011976 maleic acid Substances 0.000 claims description 5
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 5
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 5
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 4
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 4
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 230000008569 process Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 238000012662 bulk polymerization Methods 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- -1 ethylene oxybutyl Chemical group 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- CPJRRXSHAYUTGL-UHFFFAOYSA-N isopentenyl alcohol Chemical compound CC(=C)CCO CPJRRXSHAYUTGL-UHFFFAOYSA-N 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011426 gypsum mortar Substances 0.000 description 1
- 238000011419 induction treatment Methods 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- 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
-
- 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
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/28—Treatment by wave energy or particle radiation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/02—Polyalkylene oxides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a preparation method of a slice type polycarboxylate water reducer, which is characterized in that polyether is subjected to microwave treatment, and then is polymerized into a high polymer at low temperature together with an initiating agent, a chain transfer agent and an active agent, and then is concentrated, solidified and sliced, so that the preparation of a solid slice type polycarboxylate water reducer is realized.
Description
Technical Field
The invention relates to the technical field of water reducer preparation, in particular to a preparation method of a slice type polycarboxylate water reducer.
Background
The water reducing agent is a concrete admixture capable of reducing the mixing water consumption under the condition of maintaining the slump of the concrete basically unchanged. The polycarboxylate water reducer is widely applied as a water reducer, and two preparation modes of spray drying and bulk polymerization are adopted in the traditional preparation method.
Spray drying processes are generally energy intensive and require special release agents and protections, which result in both cost and water reducing agent properties being affected. The self-polymerization reaction is easy to occur in the bulk polymerization, and the performance of the water reducer is seriously affected.
Disclosure of Invention
The invention provides a preparation method of a high-performance slice type polycarboxylate superplasticizer, which comprises the following steps of:
step 1: carrying out low-temperature microwave treatment on polyether;
step 2: cooling the treated polyether;
step 3: introducing the cooled polyether into a reaction kettle, and simultaneously dripping an initiator, a chain transfer agent and an active agent to realize low-temperature polymerization;
step 4: taking out the high polymer after low-temperature polymerization and concentrating at low temperature;
step 5: drying the concentrated high molecular polymer at a low temperature, cooling and solidifying to finish the preparation of the polycarboxylate water reducer;
step 6: slicing the cured polycarboxylate superplasticizer.
In the step 1, the temperature of the low-temperature microwave treatment is 5-25 ℃ and the time is 2-5 minutes.
Further, in the step 2, the temperature of the polyether subjected to the low-temperature microwave treatment is reduced by 10-15 ℃ through heat exchange treatment, and the polyether can be one of vinyl polyethylene glycol ether, ethylene oxybutyl polyethylene glycol ether, isopentenyl alcohol polyoxyethylene ether, isobutenyl alcohol polyoxyethylene ether and allyl alcohol polyoxyethylene ether.
Further, in the step 3, the initiator is hydrogen peroxide; the chain transfer agent is one or more of mercaptopropionic acid, mercaptoacetic acid or hypophosphite; the active agent is one or more of acrylic acid, itaconic acid and maleic acid.
Further, in the step 3, the mixture continuously flows back in the low-temperature polymerization process in the reaction kettle, so that the alternate operation of cooling and microwave treatment is realized.
Further, in step 3, the mixture is reacted to a high molecular polymer with a concentration of 40% -60% in the reaction kettle.
Compared with the prior art, the invention has the advantages that:
1. compared with 40-60% aqueous solution polymerized polycarboxylate water reducer, the microwave-induced polyether has higher activation energy, can more easily generate homopolymerization reaction with acrylic acid, itaconic acid and maleic acid at low temperature, and has narrower molecular weight distribution and fewer impurities through the subsequent induction treatment of specific microwaves.
2. Compared with the polycarboxylate water reducer obtained by spray drying or bulk polymerization, the polycarboxylate water reducer has fewer impurities and better water reducing and slump retaining performances.
3. The process adopts low-temperature drying to form massive solid, then slicing, no dust is generated in the process, and the generated water is further recycled to prepare the polycarboxylate water reducer with low concentration for sale in the nearby market. The enterprises can realize circular economy, low carbon and environmental protection.
4. The product of the product is solid sheet, can be packaged by plastic bags and kraft paper, is simple to package, and the packaging material can be recycled. Compared with the traditional liquid water reducing agent, the transportation cost of the solid is saved by 50 percent. Low carbon and economy.
5. Compared with the 50% concentration liquid polycarboxylate water reducer which can only be used for concrete additives, the slice solid polycarboxylate water reducer can be used in dry environments such as dry powder mortar, gypsum mortar and the like, and the application field of products is effectively widened.
Drawings
FIG. 1 is a flow chart of a method for preparing a polycarboxylate superplasticizer of example 1 of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be further described below.
Example 1:
as shown in fig. 1, the invention provides a preparation method of a slice type polycarboxylate superplasticizer, which comprises the following steps:
step 1: carrying out low-temperature microwave treatment on polyether; the temperature of the low-temperature microwave treatment is 15 ℃; the time is 3 minutes, the polyether activity is improved by 3-5%, the microwave power is controlled to be 3 kilowatts, the microwave-induced polyether activation energy is higher, the homopolymerization reaction with acrylic acid, itaconic acid and maleic acid can be more easily generated at low temperature, and the molecular weight distribution of the polycarboxylate water reducer is narrower and the impurities are less through the induction subsequent treatment of specific microwaves.
Step 2: cooling the treated polyether by heat exchange at 10 ℃, then cooling the polyether, and then introducing the polyether into a reaction kettle;
in this embodiment, the temperature of polyether is mainly reduced through low temperature heat exchange treatment, and the reaction kettle is connected with the low temperature microwave treatment device through a conveying pipeline, and the outside of the conveying pipeline can be subjected to heat exchange treatment through liquid such as water, so that the temperature of polyether is reduced.
Step 3: weighing the components according to the proportion of the raw materials, putting polyether serving as a bottom material into a reaction kettle, and simultaneously dripping an initiator, a chain transfer agent and an active agent to realize low-temperature polymerization; in this embodiment, the initiator is hydrogen peroxide; the chain transfer agent is mercaptopropionic acid; the active agent is acrylic acid, and the concentration of the polymerized high molecular polymer is 40% -60%. The low-temperature polymerization reaction in the aqueous solution ensures that the reaction is a homopolymerization reaction, and reduces the self-polymerization of small molecules to cause poor performance of the final product.
The reaction kettle adopted in the step 3 comprises a reaction kettle, a heat exchanger, a microwave processor, a stirrer, a circulating pipeline, a valve and a circulating pump; the microwave processor and the stirrer are arranged in the reaction kettle, the feeding hole of the circulating pipeline is inserted from the bottom of the reaction kettle, the discharging hole of the microwave processor is inserted from the top of the reaction kettle, the circulating pipeline is provided with a circulating pump and a valve, and the circulating pipeline exchanges heat by arranging heat exchange equipment.
Under the action of a circulating pump, the high molecular polymer in the kettle is continuously mixed: the cycle process of microwave heating, heat exchange cooling and microwave heating again is that in this embodiment, the cycle number is: 3 times, the microwave power is controlled to be 20-50 kilowatts, and the temperature of low-temperature microwave treatment is 20-30 ℃; the temperature of the high polymer is increased by 5-8 ℃ each time, the polyether activity is increased by 30-50%, and the heat of chemical reaction and microwave treatment is taken away by a circulating heat exchanger each time, so that the high polymer in the kettle is ensured to carry out polymerization reaction at the temperature of not higher than 30 ℃.
Step 4: taking out the high polymer after low-temperature polymerization, concentrating at low temperature of not higher than 40 ℃, vacuumizing, concentrating from 40% -60% to 75-80%, and facilitating the next low-temperature microwave drying; in the concentration process, the molecular weight of the polycarboxylate water reducer is further processed and distributed under the induction of specific microwaves, so that the molecular weight distribution is narrower (from 92-95% to 95-98%), and the impurity content is further reduced by 3-4% to 1.5-2.0%.
Step 5: drying 75-80% of the concentrated high polymer at low temperature, cooling and solidifying to prepare the polycarboxylate water reducer; the concentrated solution enters a belt dryer for drying treatment, the belt dryer is composed of a main evaporation area, a mild evaporation area and a cooling area, and the device cylinder body is divided into a plurality of functional areas. The front section of the feeding end is a main evaporation area, microwave power is intensive, the high polymer enters a stable evaporation section after being evaporated to the water content of 90-95%, the temperature of the stable evaporation section is 30 ℃, the water content is reduced to below 0.5% for cooling and solidifying, a cooling plate is arranged at the discharging section, and the materials are cooled to the solidifying and cooling temperature, so that the crushing of cake-shaped dry materials by the crusher in the discharging end is facilitated. The microwave power, temperature and vacuum degree corresponding to each interval are adjusted according to the actual condition of the water content, and the microwave power and the vacuum degree are adjusted through embedding of the temperature and humidity sensors, so that the temperature and the vacuum degree are accurately controlled. The number of layers of the crawler belt is 8-15, the concentrated high polymer is automatically added, the speed of each layer of the crawler belt can be adjusted in a variable frequency and stepless manner, and the crawler belt is independently adjustable and is produced in a digital and full-automatic manner.
Step 6: and slicing the cured polycarboxylate superplasticizer to prepare a sample 4.
Example 2:
the preparation method of the slice type polycarboxylate superplasticizer comprises the following steps of:
step 1: carrying out low-temperature microwave treatment on polyether; the temperature of the low-temperature microwave treatment is 25 ℃; the time is 5 minutes, the polyether activity is improved by 4%, the microwave power is controlled to be 3-8 kilowatts, the microwave-induced polyether activation energy is higher, the homopolymerization reaction with acrylic acid, itaconic acid and maleic acid can be more easily generated at low temperature, and the molecular weight distribution of the polycarboxylate water reducer is narrower and the impurities are less through the induction subsequent treatment of specific microwaves.
Step 2: cooling the treated polyether by heat exchange at 15 ℃, and then introducing the polyether into a reaction kettle;
in this embodiment, the temperature of polyether is mainly reduced through low temperature heat exchange treatment, and the reaction kettle is connected with the low temperature microwave treatment device through a conveying pipeline, and the outside of the conveying pipeline can be subjected to heat exchange treatment through liquid such as cooling circulating water, so that the temperature of polyether is reduced.
Step 3: weighing the components according to the proportion of the raw materials, putting polyether serving as a bottom material into a reaction kettle, and simultaneously dripping an initiator, a chain transfer agent and an active agent to realize low-temperature polymerization; in this embodiment, the initiator is hydrogen peroxide; the chain transfer agent is mercaptopropionic acid; the active agent is acrylic acid, and the concentration of the polymerized high polymer is 40-60%. The low-temperature polymerization reaction in the aqueous solution ensures that the reaction is a homopolymerization reaction, and reduces the self-polymerization of small molecules to cause poor performance of the final product.
The reaction kettle adopted in the step 3 comprises a reaction kettle, a heat exchanger, a microwave processor, a stirrer, a circulating pipeline, a valve and a circulating pump; the microwave processor and the stirrer are arranged in the reaction kettle, the feeding hole of the circulating pipeline is inserted from the bottom of the reaction kettle, the discharging hole of the microwave processor is inserted from the top of the reaction kettle, and the circulating pipeline is provided with a circulating pump and a valve.
Under the action of a circulating pump, the high molecular polymer in the kettle is continuously mixed: the cycle process of microwave heating, heat exchange cooling and microwave heating again is that in this embodiment, the cycle number is: 3 times, the microwave power is 15 kilowatts, and the temperature of low-temperature microwave treatment is 20 ℃; the temperature of the high polymer rises by 5 ℃ in the process of entering the reaction kettle to being discharged from the reaction kettle every time of circulation, the polyether activity is improved by 50%, and the heat of chemical reaction and microwave treatment is taken away by a circulation heat exchanger every time of circulation, so that the high polymer in the kettle is ensured to carry out polymerization reaction under the condition of not higher than 30 ℃.
Step 4: taking out the high polymer after low-temperature polymerization, concentrating at low temperature of not higher than 40 ℃, vacuumizing, concentrating from 40-60% to 75-80%, and facilitating the next low-temperature microwave drying; in the concentration process, the molecular weight of the polycarboxylate water reducer is further processed and distributed under the induction of specific microwaves, so that the molecular weight distribution is narrower (from 92-95% to 95-98%), and the impurity content is further reduced by 3-4% to 1.5-2.0%.
Step 5: drying 75-80% of the concentrated high polymer at low temperature, cooling and solidifying to prepare the polycarboxylate water reducer; the concentrated solution enters a belt dryer for drying treatment, the belt dryer is composed of a main evaporation area, a mild evaporation area and a cooling area, and the device cylinder body is divided into a plurality of functional areas. The front section of the feeding end is a main evaporation area, microwave power is intensive, the high polymer enters a stable evaporation section after being evaporated to the water content of 90-95%, the temperature of the stable evaporation section is 50 ℃, the rear section is mainly the stable evaporation, the water content is reduced to below 0.5%, cooling solidification is carried out, a cooling plate is arranged at the discharging section, the materials are cooled to the solidification and friable temperature, and the crushing of cake-shaped dry materials by the crusher in the discharging end is facilitated. The microwave power, temperature and vacuum degree corresponding to each interval are adjusted according to the actual condition of the water content, and the microwave power and the vacuum degree are adjusted through embedding of the temperature and humidity sensors, so that the temperature and the vacuum degree are accurately controlled. The number of layers of the crawler belt is 8-15, the concentrated high polymer is automatically added, the speed of each layer of the crawler belt can be adjusted in a variable frequency and stepless manner, and the crawler belt is independently adjustable and is produced in a digital and full-automatic manner.
Step 6: and slicing the cured polycarboxylate superplasticizer to prepare a sample 5.
To further discuss the technical effects of the present invention, the present invention is discussed by comparing sample 4 prepared in example 1, sample 5 prepared in example 2 with sample 1, sample 2 of the prior art and sample 3 without microwave treatment, microwave drying solids.
The experimental cement is conch 42.5 cement, and the fly ash is Wanergy secondary ash. The mud content is 1.8%, and the fineness modulus is 2.6. 1.0% of mud and 5-25 particle size. Stirring time is 180 seconds, and vibrating time is 15 seconds. The mixing ratio is cement: fly ash: sand: stone: water = 300:100:773:1067:160. the blending amount of the water reducing agent is folded and fixed. 0.15%.
Concrete performance test results with attached table
Sample 1 (commercially available, spray-dried), sample 2 (commercially available, bulk polymerized), sample 3 (homemade, 50% aqueous solution polymerized) and sample 4 (homemade, 50% aqueous solution polymerized, microwave treated, microwave dried) were tested for concrete, parallel comparative tests with the same raw materials, the same concrete mix ratios, samples 1, 2, 3, 4 and 5 were tested with the same solids content and the same mix amount, and from the test results it can be seen that the initial slump, expansion, or slump, expansion loss over time of freshly mixed concrete of homemade, 50% aqueous solution polymerized, microwave treated, microwave dried solids were superior to those of commercially available spray-dried, bulk polymerized and homemade raw materials without low temperature microwave treatment, low temperature microwave and low temperature microwave concentrated polycarboxylate water reducer used in polymerization.
The foregoing is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any person skilled in the art will make any equivalent substitution or modification to the technical solution and technical content disclosed in the invention without departing from the scope of the technical solution of the invention, and the technical solution of the invention is not departing from the scope of the invention.
Claims (7)
1. The preparation method of the slice type polycarboxylate superplasticizer is characterized by comprising the following steps of:
step 1: carrying out low-temperature microwave treatment on polyether;
step 2: cooling the treated polyether;
step 3: introducing the polyether after cooling into a reaction kettle, and simultaneously dripping an initiator, a chain transfer agent and an active agent to realize low-temperature polymerization;
step 4: taking out the high polymer after low-temperature polymerization and concentrating at low temperature;
step 5: drying the concentrated high molecular polymer at a low temperature, cooling and solidifying to finish the preparation of the polycarboxylate water reducer;
step 6: slicing the cured polycarboxylate superplasticizer.
2. The method for preparing a chip polycarboxylate superplasticizer as recited in claim 1, wherein in step 1, the temperature of the low-temperature microwave treatment is 5-25 ℃ for 2-5 minutes.
3. The method for preparing a chip polycarboxylate superplasticizer as recited in claim 1, wherein in step 2, the polyether after low temperature microwave treatment is cooled by 10-15 ℃ through heat exchange treatment.
4. The method for preparing a slice type polycarboxylate superplasticizer as recited in claim 1, wherein in step 3, the initiator is hydrogen peroxide; the chain transfer agent is one or more of mercaptopropionic acid, mercaptoacetic acid or hypophosphite; the active agent is one or more of acrylic acid, itaconic acid and maleic acid.
5. The method for preparing the slice type polycarboxylate superplasticizer as claimed in claim 1, wherein in step 3, the mixture continuously flows back in the low temperature polymerization process in the reaction kettle, so as to realize the alternate operation of cooling and microwave treatment, the temperature of the mixture treated in the reaction kettle is increased by 5 ℃ after each round of backflow, and the high molecular polymer in the reaction kettle is polymerized at the temperature of not higher than 30 ℃.
6. The method for preparing a chip polycarboxylate superplasticizer as recited in claim 1, wherein in step 3, the mixture is reacted into a polymer having a concentration of 40% -60% in the reaction vessel.
7. The method for preparing a chip polycarboxylate water reducing agent according to claim 1, wherein in step 5, the high polymer after concentration is evaporated to a water content of 90-95% and then enters a stationary evaporation section, the temperature of the stationary evaporation section is 20-50 ℃, and the water content is below 0.5%, and then cooling and solidifying are performed.
Priority Applications (1)
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