CN107759746A - The synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent - Google Patents
The synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent Download PDFInfo
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- CN107759746A CN107759746A CN201710962185.8A CN201710962185A CN107759746A CN 107759746 A CN107759746 A CN 107759746A CN 201710962185 A CN201710962185 A CN 201710962185A CN 107759746 A CN107759746 A CN 107759746A
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- deionized water
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- reducing 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
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
A kind of synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent, synthesis step are：(1) reactor adds deionized water and methyl allyl alcohol polyoxyethylene ether, is heated with stirring to 60 ± 2 DEG C；(2) solution is prepared 1.：Deionized water+ascorbic acid+mercaptopropionic acid；Prepare solution 2.：Deionized water+acrylic acid；(3) solution is prepared 3.：Deionized water+ascorbic acid+mercaptopropionic acid；Prepare solution 4.：Deionized water+acrylic acid；(4) step (1) adds hydrogen peroxide, uniformly drip respectively above-mentioned steps (2) preparation 1., 2. number solution；Do not drip prepared by above-mentioned rapid (3) then 3., 4. solution；(5) aging reaction 60 minutes；(6) liquid caustic soda for being cooled to less than 45 DEG C 30% sodium hydroxides of addition is neutralized to pH6 or so；Beneficial effect is：Production cycle shortened about 3 hours till now from original 5~6 hours, product qualification rate by original 80~90% improve till now 100%.
Description
Technical field
The present invention relates to a kind of concrete additive, and in particular to a kind of synthesis of collapse protective poly-carboxylic acid high-performance water reducing agent
Method.
Background technology
Existing high performance water reducing agent of polyocarboxy acid synthesis is all that polymerisation in solution is carried out under normal pressure and certain temperature, some polymerizations
Monomer was uniformly dripped at 3 hours or so mostly, and then aging certain time, supply and demand 5~6 are small at a certain temperature again
When, production cycle length, low production efficiency unstable product quality, product qualification rate only has 80~90%.
The content of the invention
It is an object of the invention to make up the deficiencies in the prior art, there is provided a kind of to make the production cycle from original 5~6 hours
Shorten about 3 hours till now, while the synthetic method of the collapse protective poly-carboxylic acid high-performance water reducing agent to improve product quality stability.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent, raw material include methyl allyl alcohol polyoxyethylene ether,
Acrylic acid, mercaptopropionic acid, hydrogen peroxide, ascorbic acid, deionized water, 30% sodium hydroxide；It is characterized in that：
Synthesis step is：
(1) reactor adds 200~300kg deionized waters and 300~400kg methyl allyl alcohol polyoxyethylene ethers, stirring
It is heated to 60 ± 2 DEG C；
(2) solution is prepared 1.：Deionized water 10~15kg+, 0.1~0.2kg+ of ascorbic acid mercaptopropionic acids 0.01~
0.02kg；Prepare solution 2.：2~3kg of deionized water 1~2kg+ acrylic acid；
(3) solution is prepared 3.：0.2~0.3kg of deionized water 100~150kg+ ascorbic acid 1~1.5kg+ mercaptopropionic acids；
Prepare solution 4.：2~3kg of deionized water 1~2kg+ acrylic acid；
(4) after the solution clarification that prepared by step (1), 1~2kg hydrogen peroxide is added, maintains the temperature at 60 ± 2 DEG C, with 10~
20 minutes uniformly drip respectively above-mentioned steps (2) preparation 1., 2. number solution；Then distinguished with 20~40 minutes
Drip prepared by above-mentioned rapid (3) 3., 4. solution；
(5) 60 DEG C of aging reactions are maintained the temperature at 60 minutes；
(6) liquid caustic soda for being cooled to less than 45 DEG C addition 20~30kg30% sodium hydroxides is neutralized to pH6 or so, obtains collapse protection type
High performance water reducing agent of polyocarboxy acid.
Compared with the prior art, the invention has the advantages that：Production cycle shortened till now about from original 5~6 hours
3 hours, product qualification rate by original 80~90% improve till now 100%.
Embodiment
The present invention is further illustrated below by embodiment.
Embodiment 1
A kind of synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent, raw material include methyl allyl alcohol polyoxyethylene ether,
Acrylic acid, mercaptopropionic acid, hydrogen peroxide, ascorbic acid, deionized water, 30% sodium hydroxide；It is characterized in that：
Synthesis step is：
(1) reactor adds 200kg deionized waters and 300kg methyl allyl alcohol polyoxyethylene ethers, is heated with stirring to 60 ± 2
℃；
(2) solution is prepared 1.：Deionized water 10kg+ ascorbic acid 0.1kg+ mercaptopropionic acids 0.01kg；Prepare solution 2.：Go
Ionized water 1kg+ acrylic acid 2kg；
(3) solution is prepared 3.：Deionized water 100kg+ ascorbic acid 1kg+ mercaptopropionic acids 0.2kg；Prepare solution 4.：Go from
Sub- water 1kg+ acrylic acid 2kg；
(4) after the solution clarification that prepared by step (1), 1kg hydrogen peroxide is added, 60 DEG C are maintained the temperature at, with 10 minutes
Uniformly drip respectively above-mentioned steps (2) preparation 1., 2. number solution；Then dripped respectively with 20 minutes above-mentioned rapid
(3) prepare 3., 4. solution；
(5) 60 DEG C of aging reactions are maintained the temperature at 60 minutes；
(6) liquid caustic soda for being cooled to less than 45 DEG C addition 20kg30% sodium hydroxides is neutralized to pH6 or so, obtains the poly- carboxylic of collapse protection type
Sour high-performance water reducing agent.
Production cycle shortened about 3 hours till now from original 5~6 hours, and product qualification rate is by original 80~90%
Improve 100% till now.
Embodiment 2
A kind of synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent, raw material include methyl allyl alcohol polyoxyethylene ether,
Acrylic acid, mercaptopropionic acid, hydrogen peroxide, ascorbic acid, deionized water, 30% sodium hydroxide；It is characterized in that：
Synthesis step is：
(1) reactor adds 300kg deionized waters and 400kg methyl allyl alcohol polyoxyethylene ethers, is heated with stirring to 60 ± 2
℃；
(2) solution is prepared 1.：Deionized water 15kg+ ascorbic acid 0.2kg+ mercaptopropionic acids 0.02kg；Prepare solution 2.：Go
Ionized water 2kg+ acrylic acid 3kg；
(3) solution is prepared 3.：Deionized water 150kg+ ascorbic acid 1.5kg+ mercaptopropionic acids 0.3kg；Prepare solution 4.：Go
Ionized water 2kg+ acrylic acid 3kg；
(4) after the solution clarification that prepared by step (1), 2kg hydrogen peroxide is added, 60 DEG C are maintained the temperature at, with 10~20 minutes
Time uniformly drip respectively above-mentioned steps (2) preparation 1., 2. number solution；Then dripped respectively with 40 minutes above-mentioned
Suddenly (3) prepare 3., 4. solution；
(5) 60 DEG C of aging reactions are maintained the temperature at 60 minutes；
(6) liquid caustic soda for being cooled to less than 45 DEG C addition 30kg30% sodium hydroxides is neutralized to pH6 or so, obtains the poly- carboxylic of collapse protection type
Sour high-performance water reducing agent.
Production cycle shortened about 3 hours till now from original 5~6 hours, and product qualification rate is by original 80~90%
Improve 100% till now.
Claims (1)
1. a kind of synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent, raw material includes methyl allyl alcohol polyoxyethylene ether, third
Olefin(e) acid, mercaptopropionic acid, hydrogen peroxide, ascorbic acid, deionized water, 30% sodium hydroxide；It is characterized in that：
Synthesis step is：
(1) reactor adds 200~300kg deionized waters and 300~400kg methyl allyl alcohol polyoxyethylene ethers, agitating and heating
To 60 ± 2 DEG C；
(2) solution is prepared 1.：0.01~0.02kg of deionized water 10~15kg+ ascorbic acid 0.1~0.2kg+ mercaptopropionic acids；System
Standby solution is 2.：2~3kg of deionized water 1~2kg+ acrylic acid；
(3) solution is prepared 3.：0.2~0.3kg of deionized water 100~150kg+ ascorbic acid 1~1.5kg+ mercaptopropionic acids；Prepare
Solution is 4.：2~3kg of deionized water 1~2kg+ acrylic acid；
(4) after the solution clarification that prepared by step (1), 1~2kg hydrogen peroxide is added, 60 ± 2 DEG C are maintained the temperature at, with 10~20 points
Clock time uniformly drip respectively above-mentioned steps (2) preparation 1., 2. number solution；Then it is added dropwise respectively with 20~40 minutes
Complete above-mentioned rapid (3) prepare 3., 4. solution；
(5) 60 DEG C of aging reactions are maintained the temperature at 60 minutes；
(6) liquid caustic soda for being cooled to less than 45 DEG C addition 20~30kg30% sodium hydroxides is neutralized to pH6 or so, obtains the poly- carboxylic of collapse protection type
Sour high-performance water reducing agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710962185.8A CN107759746A (en) | 2017-10-08 | 2017-10-08 | The synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent |
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| CN201710962185.8A CN107759746A (en) | 2017-10-08 | 2017-10-08 | The synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018397A (en) * | 2019-12-02 | 2020-04-17 | 浙江天造环保科技有限公司 | High slump loss resistant type polycarboxylic acid high-performance water reducing agent and preparation method thereof |
| CN111018396A (en) * | 2019-12-02 | 2020-04-17 | 浙江天造环保科技有限公司 | Antirust high slump loss resistant polycarboxylic acid high-performance water reducing agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951866A (en) * | 2012-06-21 | 2013-03-06 | 马清浩 | Ascorbic acid modified carboxylic water reducer and preparation method thereof |
| CN104987469A (en) * | 2015-06-30 | 2015-10-21 | 同济大学 | Preparing method for high dispersion type polycarboxylate water reducing agent |
-
2017
- 2017-10-08 CN CN201710962185.8A patent/CN107759746A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951866A (en) * | 2012-06-21 | 2013-03-06 | 马清浩 | Ascorbic acid modified carboxylic water reducer and preparation method thereof |
| CN104987469A (en) * | 2015-06-30 | 2015-10-21 | 同济大学 | Preparing method for high dispersion type polycarboxylate water reducing agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018397A (en) * | 2019-12-02 | 2020-04-17 | 浙江天造环保科技有限公司 | High slump loss resistant type polycarboxylic acid high-performance water reducing agent and preparation method thereof |
| CN111018396A (en) * | 2019-12-02 | 2020-04-17 | 浙江天造环保科技有限公司 | Antirust high slump loss resistant polycarboxylic acid high-performance water reducing agent and preparation method thereof |
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Application publication date: 20180306 |