CN108219045A - A kind of collapse protection type high efficiency water reducing agent and its production technology - Google Patents

A kind of collapse protection type high efficiency water reducing agent and its production technology Download PDF

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Publication number
CN108219045A
CN108219045A CN201611187441.2A CN201611187441A CN108219045A CN 108219045 A CN108219045 A CN 108219045A CN 201611187441 A CN201611187441 A CN 201611187441A CN 108219045 A CN108219045 A CN 108219045A
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China
Prior art keywords
reducing agent
high efficiency
water
type high
protection type
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CN201611187441.2A
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Chinese (zh)
Inventor
陈国杰
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Yibin Jiete Manchester Building Materials Co Ltd
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Yibin Jiete Manchester Building Materials Co Ltd
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Priority to CN201611187441.2A priority Critical patent/CN108219045A/en
Publication of CN108219045A publication Critical patent/CN108219045A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/04Acids; Metal salts or ammonium salts thereof
    • C08F120/06Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/38Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers

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  • 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)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The present invention provides a kind of production technology of collapse protection type high efficiency water reducing agent, it is characterised in that:Include the following steps;S1:Water, ether, acrylic acid, hydrogen peroxide are uniformly mixed and S1 solution are obtained by the reaction;S2:Acrylic acid, which is added to the water to be uniformly mixed, obtains A material;Thioacetic acid, which is added to the water to be uniformly mixed, obtains B material;S3:A is expected, B material are added drop-wise in S1 solution and react respectively, obtain S3 solution;S4:It is 67 that aqueous slkali is added in S3 solution and adjusts PH, continues stirring 15 25 minutes.The water-reducing agent obtained using above-mentioned preparation method can effectively extend the water-reducing rate protected and water-reducing agent can be also promoted while collapsing the time.

Description

A kind of collapse protection type high efficiency water reducing agent and its production technology
Technical field
The present invention relates to a kind of water-reducing agent and its production technology, more particularly to a kind of collapse protection type high efficiency water reducing agent and its production Technique.
Background technology
Slump retaining agent and water-reducing agent are all common materials in construction material, for being added in concrete to the object of concrete Rationality matter is adjusted, and wherein slump retaining agent causes concrete set time to slow down, and water-reducing agent may be such that the moisture in concrete subtracts Few, the additive that batched water can be greatly reduced under conditions of concrete slump is essentially identical is known as high efficiency water reducing agent. There was only simple slump retaining agent or water-reducing agent/high efficiency water reducing agent in the market earliest, simple slump retaining agent guarantor is collapsed, and effect is poor, and guarantor is collapsed Time generally at 1-1.5 hours, will start to solidify more than this time concrete, be not easy to long-distance long-time transport, Once solidification occurs in transportational process in concrete to be attached to inside bulk cement carrier, gently then reduce tank car capacity, concrete without Method is poured out, and heavy then entire concrete tank is scrapped.To solve the above problems, then there is the production containing slump retaining agent and water-reducing agent simultaneously Product.
But existing product cannot merge the effect of slump retaining agent and water-reducing agent well, and guarantor is collapsed, and the time is shorter, and transportation range is short, The few bleeding that at most can only achieve 27% existing product simultaneously of traditional water-reducing agent water-reducing rate is big simultaneously, and bleeding conference causes Grab the generation of bottom phenomenon (concrete, which is attached to inside concrete tank, to be poured out).
Therefore, it is that those skilled in the art will that guarantor is contained while how obtaining functional to collapse with the product of buck function It solves the problems, such as.
Invention content
First purpose of the present invention is to provide a kind of collapse protection type high efficiency water reducing agent and its production technology, it is therefore an objective to solve existing There is technical problem, a kind of high efficiency water reducing agent for having both slump retaining agent and water-reducing agent effect is provided.The water-reducing agent can effectively extend guarantor and collapse The water-reducing rate of water-reducing agent can be also promoted while time.
Second object of the present invention is to provide a kind of water-reducing agent prepared using above-mentioned technique.
It is of the present invention solve the problems, such as the technical solution adopted is that:
The production technology of collapse protection type high efficiency water reducing agent, includes the following steps;
S1:Water, ether are added in reaction kettle, is uniformly mixed, is added acrylic acid and be stirring evenly and then adding into hydrogen peroxide, is mixed Uniformly, S1 solution is obtained.
S2:Acrylic acid, which is added to the water to be uniformly mixed, obtains A material;Thioacetic acid, which is added to the water to be uniformly mixed, obtains B material.
S3:A is expected, B material are added drop-wise in S1 solution and react respectively, obtain S3 solution;Wherein A material start to drip in B material Start to be added dropwise after adding 2-5 minutes, and A material were dripped at 30 minutes 2 hours, B material were dripped at 30 minutes 2 hours, were added in and were completed After continue stirring 15-20 minutes.A expects, B material compare, and the prior art extends time for adding, makes reaction more abundant, and then make The water-reducing agent finally obtained has good performance.
S4:It is 6-7 that aqueous slkali is added in S3 solution and adjusts PH, continues stirring 15-25 minutes, moisturizing is to filling up reaction kettle.
Further, temperature is controlled in 20-45 degree in the S1 reaction process.
In the S1 steps, the mass ratio of each component of addition is water:Ether:Acrylic acid:Hydrogen peroxide=175-190: 170-190:1.5-2.5:0.5-1.5。
Preferably, water:Ether:Acrylic acid:Hydrogen peroxide=180-185:175-185:1.8-2.2:0.8-1.2.
In A material, each component mass ratio of addition is acrylic acid:Water=0.8-1:3.5-4.
In B material, each component mass ratio of addition is mercaptoethanol:Water=0.8-1.2:180-220.
Further, since A material and B expect too early or prepare too late cause to react insufficient, product quality is influenced, because This controls the time that it is prepared.Limit A material, B material are prepared for 15 minutes before use.
Further, it if since A material, B expect that time for adding is long or it is insufficient resolutely to cause to chemically react, influences to produce The quality of product, therefore limit the time for adding error that A expects, B expects and must not exceed ± 5 minutes.
Temperature control is at 38 degree ± 2 degree in S3 reaction process.
Collapse protection type high efficiency water reducing agent is prepared using the production technology of aforementioned collapse protection type high efficiency water reducing agent.
Beneficial effects of the present invention:
By the time lengthening expected A, B drops add in the present invention, make entirely to react more abundant, obtained product has Following superperformance:
1st, the water-reducing rate of water-reducing agent is promoted.
2nd, the mobility of concrete is increased.
3rd, extend to protect and collapse the time.
4th, reducing bleeding prevents from grabbing the generation of bottom phenomenon.
5th, the intensity of concrete is improved.
Specific embodiment
The present invention is described in further details below in conjunction with specific embodiment.
The production technology of collapse protection type high efficiency water reducing agent, includes the following steps;
S1 adds in water, ether in reaction kettle, is uniformly mixed, adds acrylic acid and be stirring evenly and then adding into hydrogen peroxide, mixes Uniformly, S1 solution is obtained.
S2, acrylic acid, which is added to the water to be uniformly mixed, obtains A material;Thioacetic acid, which is added to the water to be uniformly mixed, obtains B material.
S3, A is expected, B material are added drop-wise in S1 solution and react respectively, obtains S3 solution;Wherein A material start to drip in B material Start to be added dropwise after adding 2-5 minutes, and A material, B material dripped respectively at 30 minutes 2 hours, continued to stir 15-20 after the completion of adding in Minute.
It is 6-7 that aqueous slkali is added in S4, S3 solution and adjusts PH, continues stirring 15-25 minutes, moisturizing is to filling up reaction kettle.
Temperature control is in 20-45 degree in the S1 reaction process.
A material, B material are prepared for 15 minutes before use.
Temperature control is at 38 degree ± 2 degree in S3 reaction process.
Specific embodiment is as follows:
Embodiment 1
S1:1800 kilograms of water is added in 5000L reaction kettles, adds 1800 kilograms of import ether, starting stirring makes second Ether dissolves, and 20 kilograms of acrylic acid are added in after dissolving and continue stirring and add 10 kilogram of 27.5% hydrogen peroxide in 10 minutes to add 20 Kg of water rinses the pipeline for adding in hydrogen peroxide, stirs 5 minutes.Entire reaction temperature control is at 45 degree.
S2:A material are dissolved in 350 public water stirrings by 92 kilograms of acrylic acid and are formulated.Since too early or party excessively causes to react It is insufficient, product quality is influenced to avoid, A material are prepared for 15 minutes before taking dropwise addition.
B material are dissolved in stirring in 500 kg of water by 2.5 kilograms of thioacetic acid and are formulated.Since too early or party excessively causes It reacts insufficient, influences product quality to avoid, B material are prepared for 15 minutes before also taking dropwise addition.
S3:Prepared A, B are expected in two measuring tanks being drawn into above reaction kettle by pipeline respectively, first extract B Add 100 kg of water flushing pipes (purpose prevents A to be mixed into B material in expecting) in material to measuring tank again, then A material are drawn into another meter In measuring tank.
Start be added dropwise A, B material, first be added dropwise B material, A material B material start be added dropwise start to be added dropwise after five minutes, B expect 2 hours 30 points Clock at the uniform velocity adds, and A expects at the uniform velocity to add for 30 minutes 2 hours, and A, B material time for adding error must not exceed ± 5 minutes.If be added dropwise Between it is long or can resolutely cause to chemically react insufficient, influence the quality of product.
Continue stirring 15 minutes after the completion of adding in, entire reaction temperature control is at 38 degree ± 2 degree.
S4:It is added dropwise after the completion of A, B material, adds in 155 kilogram of 32% liquid caustic soda and neutralize, pH value is controlled between 6-7, continues to stir 300 kilograms of moisturizing (filling up reaction kettle volume) can discharge after 15 minutes.
Embodiment 2
S1:1750 kilograms of water is added in 5000L reaction kettles, adds 1700 kilograms of import ether, starting stirring makes second Ether dissolves, and 15 kilograms of acrylic acid are added in after dissolving and continue stirring and add 5 kilogram of 27.5% hydrogen peroxide in 10 minutes to add 20 Kg of water rinses the pipeline for adding in hydrogen peroxide, stirs 5 minutes.Entire reaction temperature control is at 20 degree.
S2:A material are dissolved in 400 public water stirrings by 80 kilograms of acrylic acid and are formulated.Since too early or party excessively causes to react It is insufficient, product quality is influenced to avoid, A material are prepared for 15 minutes before taking dropwise addition.
B material are dissolved in stirring in 450 kg of water by 2.4 kilograms of thioacetic acid and are formulated.Since too early or party excessively causes It reacts insufficient, influences product quality to avoid, B material are prepared for 15 minutes before also taking dropwise addition.
S3:Prepared A, B are expected in two measuring tanks being drawn into above reaction kettle by pipeline respectively, first extract B Add 100 kg of water flushing pipes (purpose prevents A to be mixed into B material in expecting) in material to measuring tank again, then A material are drawn into another meter In measuring tank.
Start be added dropwise A, B material, first be added dropwise B material, A material B material start be added dropwise 3 minutes after start to be added dropwise, B expect 2 hours 30 points Clock at the uniform velocity adds, and A expects at the uniform velocity to add for 30 minutes 2 hours, and A, B material time for adding error must not exceed ± 5 minutes.If be added dropwise Between it is long or can resolutely cause to chemically react insufficient, influence the quality of product.
Continue stirring 20 minutes after the completion of adding in, entire reaction temperature control is at 38 degree ± 2 degree.
S4:It is added dropwise after the completion of A, B material, adds in 155 kilogram of 32% liquid caustic soda and neutralize, pH value is controlled between 6-7, continues to stir Moisturizing can discharge to reaction kettle is filled up after 15 minutes.
Embodiment 3
S1:1900 kilograms of water is added in 5000L reaction kettles, adds 1850 kilograms of import ether, starting stirring makes second Ether dissolves, and 25 kilograms of acrylic acid are added in after dissolving and continue stirring and add 12 kilogram of 27.5% hydrogen peroxide in 10 minutes to add 20 Kg of water rinses the pipeline for adding in hydrogen peroxide, stirs 5 minutes.Entire reaction temperature control is at 30 degree.
S2:A material are dissolved in 350 public water stirrings by 80 kilograms of acrylic acid and are formulated.Since too early or party excessively causes to react It is insufficient, product quality is influenced to avoid, A material are prepared for 15 minutes before taking dropwise addition.
B material are dissolved in stirring in 500 kg of water by 2.3 kilograms of thioacetic acid and are formulated.Since too early or party excessively causes It reacts insufficient, influences product quality to avoid, B material are prepared for 15 minutes before also taking dropwise addition.
S3:Prepared A, B are expected in two measuring tanks being drawn into above reaction kettle by pipeline respectively, first extract B Add 100 kg of water flushing pipes (purpose prevents A to be mixed into B material in expecting) in material to measuring tank again, then A material are drawn into another meter In measuring tank.
Start be added dropwise A, B material, first be added dropwise B material, A material B material start be added dropwise 4 minutes after start to be added dropwise, B expect 2 hours 30 points Clock at the uniform velocity adds, and A expects at the uniform velocity to add for 30 minutes 2 hours, and A, B material time for adding error must not exceed ± 5 minutes.If be added dropwise Between it is long or can resolutely cause to chemically react insufficient, influence the quality of product.
Continue stirring 20 minutes after the completion of adding in, entire reaction temperature control is at 38 degree ± 2 degree.
S4:It is added dropwise after the completion of A, B material, adds in 155 kilogram of 32% liquid caustic soda and neutralize, pH value is controlled between 6-7, continues to stir Moisturizing can discharge to reaction kettle is filled up after 15 minutes.
Embodiment 4
S1:1850 kilograms of water is added in 5000L reaction kettles, adds 1750 kilograms of import ether, starting stirring makes second Ether dissolves, and 18 kilograms of acrylic acid are added in after dissolving and continue stirring and add 8 kilogram of 27.5% hydrogen peroxide in 10 minutes to add 20 Kg of water rinses the pipeline for adding in hydrogen peroxide, stirs 5 minutes.Entire reaction temperature control is at 25 degree.
S2:A material are dissolved in 350 public water stirrings by 92 kilograms of acrylic acid and are formulated.Since too early or party excessively causes to react It is insufficient, product quality is influenced to avoid, A material are prepared for 15 minutes before taking dropwise addition.
B material are dissolved in stirring in 500 kg of water by 2.5 kilograms of thioacetic acid and are formulated.Since too early or party excessively causes It reacts insufficient, influences product quality to avoid, B material are prepared for 15 minutes before also taking dropwise addition.
S3:Prepared A, B are expected in two measuring tanks being drawn into above reaction kettle by pipeline respectively, first extract B Add 100 kg of water flushing pipes (purpose prevents A to be mixed into B material in expecting) in material to measuring tank again, then A material are drawn into another meter In measuring tank.
Start be added dropwise A, B material, first be added dropwise B material, A material B material start be added dropwise start to be added dropwise after five minutes, B expect 2 hours 30 points Clock at the uniform velocity adds, and A expects at the uniform velocity to add for 30 minutes 2 hours, and A, B material time for adding error must not exceed ± 5 minutes.If be added dropwise Between it is long or can resolutely cause to chemically react insufficient, influence the quality of product.
Continue stirring 15 minutes after the completion of adding in, entire reaction temperature control is at 38 degree ± 2 degree.
S4:It is added dropwise after the completion of A, B material, adds in 155 kilogram of 32% liquid caustic soda and neutralize, pH value is controlled between 6-7, continues to stir Moisturizing can discharge to reaction kettle is filled up after 15 minutes.
Comparative example
Except the time for adding of A material, B material is 1 hour, other operating process are same as Example 1, obtain water-reducing agent.
The comparison of water-reducing agent performance in table 1 to be obtained in embodiment 1-3 and comparative example.
The effect of present invention being can be seen that from the result in table 1 while having merged slump retaining agent and high efficiency water reducing agent, when guarantor is collapsed Between can extend to 2-2.5 hours, greatly extend haulage time, meet concrete long-distance transport requirement.Subtract simultaneously Water rate can reach 30%-35% so that the mobility of concrete is stronger, is more convenient tank car discharging.The present invention is mixed with being added to Can be so that the wrapping property of concrete be more preferable after solidifying soil, more abundant with the contact of rubble or cobble, small bleeding is not in grab Bottom phenomenon, and the intensity bigger of the concrete after solidification.

Claims (10)

1. the production technology of collapse protection type high efficiency water reducing agent, it is characterised in that:Include the following steps;
S1:Water, ether are added in reaction kettle, is uniformly mixed, acrylic acid is added and is stirring evenly and then adding into hydrogen peroxide, mixing is equal It is even, obtain S1 solution;
S2:Acrylic acid, which is added to the water to be uniformly mixed, obtains A material;Thioacetic acid, which is added to the water to be uniformly mixed, obtains B material;
S3:A is expected, B material are added drop-wise in S1 solution and react respectively, obtain S3 solution;Wherein A material in B material start that 2-5 is added dropwise Start to be added dropwise after minute, and A material were dripped at 30 minutes 2 hours, B material were dripped at 30 minutes 2 hours, after the completion of adding in were continued Stirring 15-20 minutes;
S4:It is 6-7 that aqueous slkali is added in S3 solution and adjusts PH, continues stirring 15-25 minutes, moisturizing.
2. the production technology of collapse protection type high efficiency water reducing agent as described in claim 1, it is characterised in that:The S1 step reactions Temperature control is in 20-45 degree in the process.
3. the production technology of collapse protection type high efficiency water reducing agent as described in claim 1, it is characterised in that:In the S1 steps, The mass ratio of each component of addition is water:Ether:Acrylic acid:Hydrogen peroxide=175-190:170-190:1.5-2.5:0.5- 1.5。
4. the production technology of collapse protection type high efficiency water reducing agent as described in claim 3, it is characterised in that:Preferably, water:Second Ether:Acrylic acid:Hydrogen peroxide=180-185:175-185:1.8-2.2:0.8-1.2.
5. the production technology of collapse protection type high efficiency water reducing agent as described in claim 1, it is characterised in that:A material in, addition it is each Constituent mass ratio is acrylic acid:Water=0.8-1:3.5-4.
6. the production technology of collapse protection type high efficiency water reducing agent as described in claim 1, it is characterised in that:B material in, addition it is each Constituent mass ratio is mercaptoethanol:Water=0.8-1.2:180-220.
7. the production technology of collapse protection type high efficiency water reducing agent as described in claim 1, it is characterised in that:A material, B material are using It prepares within first 15 minutes.
8. the production technology of collapse protection type high efficiency water reducing agent as described in claim 1, it is characterised in that:The dropwise addition of A material, B material Time error must not exceed ± 5 minutes.
9. the production technology of collapse protection type high efficiency water reducing agent as described in claim 1, it is characterised in that:The reaction of S3 steps Temperature control is at 38 degree ± 2 degree in journey.
10. collapse protection type high efficiency water reducing agent, using the production work of collapse protection type high efficiency water reducing agent such as according to any one of claims 1-8 Skill is prepared.
CN201611187441.2A 2016-12-21 2016-12-21 A kind of collapse protection type high efficiency water reducing agent and its production technology Pending CN108219045A (en)

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CN102731730A (en) * 2012-06-21 2012-10-17 马清浩 Hydrogen peroxide auxiliarily-initiated carboxylic acid water reducer and its preparation method
CN103964731A (en) * 2014-04-30 2014-08-06 山西恒泰伟业建材有限公司 Polycarboxylic acid water reducer and preparation method thereof
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CN102030494A (en) * 2010-11-12 2011-04-27 河北金舵建材科技开发有限公司 High-performance polycarboxylate water reducing agent and low-temperature one-step preparation method thereof
CN102731730A (en) * 2012-06-21 2012-10-17 马清浩 Hydrogen peroxide auxiliarily-initiated carboxylic acid water reducer and its preparation method
CN103964731A (en) * 2014-04-30 2014-08-06 山西恒泰伟业建材有限公司 Polycarboxylic acid water reducer and preparation method thereof
CN105884979A (en) * 2016-04-08 2016-08-24 湖南铭煌科技发展有限公司 Normal-temperature preparation method of slow-release polycarboxylic acid slump retaining agent
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